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1.
B. Sridhar K. Ravikumar H. Krishnan A. N. Singh 《Journal of chemical crystallography》2011,41(3):291-296
Abstract
Crystal structures of anti-migraine drug almotriptan were crystallized with oxalic acid (I) and with terephthalic acid (II) and their crystal structures and molecular associations were determined using X-ray diffraction methods. Crystals of both (I) and (II) are monoclinic, space group P21/c, with a = 5.6270(4) ?, b = 27.6419(19) ?, c = 13.6228(9) ?, β = 93.057(1)°, V = 2115.9(3) ?3, Z = 4 (I) and a = 13.3756(15) ?, b = 15.6065(17) ?, c = 10.7238(12) ?, β = 98.017(2)°, V = 2216.7(4) ?3, Z = 4 (II). In almotriptan oxalate {systematic name: N,N-dimethyl-2-[5-(pyrrolidin-1-ylsulfonyl-methyl)-1H-indol-3-yl]-ethanaminium semioxalate}, C17H26N3O2S+, C2HO4 −, (I) and in almotriptan hemi terephthalate hydrate {systematic name: N,N-dimethyl-2-[5-(pyrrolidin-1-ylsulfonyl-methyl)-1H-indol-3-yl]-ethanaminium hemi terephthalate monohydrate}, C17H26N3O2S+, 0.5(C8H4O4 2−), H2O, (II), both the almotriptan cations form a trimer with the corresponding anions via N–H···O hydrogen bonds. In (I), the oxalate salt is monoprotonated and in (II), the terephthalic acid is located across the inversion centre and exists as doubly protonated anion. In (I), the cation and anion are interlinked by the N–H···O and O–H···O hydrogen bonds into continuous two-dimensional layers generate an R66(34) hydrogen-bonded motif tetramers running parallel to the (0 0 1) plane. In (II), the cation and water form a centrosymmetric tetramer of R44(22) hydrogen-bonded motif via N–H···O and O–H···O hydrogen bonds and further cross-linked by centrosymmetric anions to form an infinite three-dimensional supramolecular hydrogen-bonded networks. 相似文献2.
Zuzana Bujdo?ová Katarína Gy?ryová Milan Melník Marian Koman Jana Ková?ová 《Journal of chemical crystallography》2011,41(4):443-448
Abstract
Two ligand isomers [Zn{4-ClC6H3-2-(OH)COO}2(Menia)2(H2O)2] (I) and [Zn{5-ClC6H3-2-(OH)COO}2(Menia)2(H2O)2] (II) (Menia = N-methylnicotinamide) were prepared and characterized by elemental analysis, IR spectroscopy and thermal analysis. The X-ray crystal structures of complexes (I) and (II) were determined. Compound (I) crystallizes in the triclinic space group P[`1] P\bar{1} with a = 8.105(1) ?, b = 10.036(2) ?, c = 10.545(2) ?, α = 109.088(9)°, β = 91.416(8)°, γ = 102.757(9)°, V = 786.2(2) ?3, Z = 1. Compound (II) crystallizes in the triclinic space group P[`1] P\bar{1} . Its cell parameters are: a = 8.133(1) ?, b = 10.119(2) ?, c = 10.428(1) ?, α = 66.44(1)°, β = 74.32(1)°, γ = 80.16(1)°, V = 755.5(2) ?3, Z = 1. The molecular structure of both isomers is monomeric. Each Zn(II) atom is hexacoordinated by three pairs of unidentate ligands in trans-positions (ZnO4N2). The 5-Clsal complex is somewhat less distorted than 4-Clsal complex (Cl-sal = chlorosalicylate). The structural data are compared with those found in similar [Zn(RCOO)2(NL)2(H2O)2]. 相似文献3.
《Journal of chemical crystallography》2011,41(7):1077-1084
Abstract
The crystal structures of two zinc(II) 4-chloro- and 5-chlorosalicylate complexes, [Zn(4-ClC6H3-2-(OH)COO)2(H2O)4]·2tph·(H2O)2 (I) and [Zn(5-ClC6H3-2-(OH)COO)2(ina)2(H2O)] (II), where tph is theophylline and ina is isonicotinamide, have been determined using X-ray diffraction methods. Crystals of both (I) and (II) are triclinic, space group P-1, with Z = 1 in a cell with a = 7.2220(3), b = 8.59700(10), c = 16.0210(5) ?, α = 75.990(2), β = 83.959(2), γ = 68.455(2)°, V = 897.54(5) ?3 (I) and with Z = 2 in a cell with a = 11.4148(11), b = 11.5327(10), c = 12.0685(13) ?, α = 63.458(6), β = 87.547(8), γ = 89.387(7)°, V = 1419.9(2) ?3 (II). The coordination environment of the zinc(II) atom of compound (I) consists of two unidentate carboxylate oxygen atoms and four oxygen atoms of aqua ligands, forming a distorted octahedral configuration. Two theophylline molecules and the remaining water molecules are bound only by hydrogen bonds. The Zn atom of compound (II) is pentacoordinated with two unidentate carboxylate oxygen atoms, two pyridine nitrogen atoms of isonicotinamide ligands, and the oxygen atom of the aqua ligand, forming a distorted configuration between square pyramid and trigonal bipyramid. In both complexes intramolecular O–H···O hydrogen-bonding interactions are present. In the crystal structures, molecules are linked by intermolecular O–H···O and N–H···O hydrogen bonds. The structures are analyzed and compared to the similar Zn(II) complexes, with the chromophores ZnO6 and ZnO3N2. 相似文献4.
Yao-Cheng Shi Hong-Jian Cheng Chun-Xia Sui Bei-Bei Zhu 《Journal of chemical crystallography》2007,37(6):399-405
Reactions of ferrocenoylacetone with thiosemicarbazide and isonicotinic acid hydrazide generate an organometallic thiosemicarbazone
1 and enehydrazide 2, respectively. The complexes 1 and 2, which can be formulated as [C5H5FeC5H4C(O)CH2C(=NNHCSNH2)CH3] and [C5H5FeC5H4C(O)CH=C(NHNHCOC5H4N-4)CH3], have been characterized by elemental analyses, IR, NMR, UV and were structurally characterized by single-crystal X-ray
crystallography.
Complex 1 (C15H17FeN3OS) crystallizes in the monoclinic space group P21/c, with lattice constants: a = 13.939(3) ?, b = 8.2600(17) ?, c = 13.176(3) ?, β = 94.83(3)°, V = 1511.7(6) ?3, Z = 4, D
c = 1.508 g cm−3, F(000) = 712, R
1 = 0.0602, wR
2 = 0.1526.
Two intermolecular hydrogen bonds N–H···S (N···S = 3.356(8) and 3.499(7) ?, N–H···S = 168 and 170°) form a chain in the [010] direction. The intermolecular hydrogen bond C–H···O (C···O = 3.432(10) ?, C–H···O = 151°)
leads to a [010] double-chain through each unit cell. The intermolecular hydrogen bond C–H···O (C···O = 3.359(10) ?, C–H···O = 173°)
makes the [010] double-chain pack along the c axis to result in a two-dimensional network.
Complex 2 (C20H19FeN3O2) crystallizes in the monoclinic space group P21/c, with lattice constants: a = 14.091(2) ?, b = 10.024(2) ?, c = 13.806(2) ?, β = 112.41(2)°, V = 1802.8(6) ?3, Z = 4, D
c = 1.434 g cm−3, F(000) = 808, R
1 = 0.0576, wR
2 = 0.1593. The strong intramolecular hydrogen bond N–H···O from the enamine N atom and carbonyl O atom stabilizes the enehydrazide.
The intermolecular hydrogen bonds N–H···O and C–H···O (N···O = 2.906(6) ?, N–H···O = 155° C···O = 3.364(6) ?, C–H···O = 153°)
generate a [010] chain.
The intermolecular hydrogen bond N–H···O (N···O = 2.989(6) ?, N–H···O = 128°) forms a [010] double-chain through each unit
cell. The π···π stacking interation involving the pyridyl groups makes the [010] double-chain pack along the c axis to lead to a two-dimensional network. 相似文献
5.
Jerry P. Jasinski Ray J. Butcher Anil N. Mayekar H. S. Yathirajan B. Narayana 《Journal of chemical crystallography》2009,39(3):157-162
Abstract In the molecular structures of three new structurally related chalcone derivatives, namely (2E)-1-(2-hydroxyphenyl)-3-(6-methoxy-2-naphthyl)prop-2-en-1-one,
C20H16O3, I, (2E)-1-(2-chloropyridin-4-yl)-3-(6-methoxy-2-naphthyl)prop-2-en-1-one, C19H14ClNO2, II, and (2E)-3-(6-methoxy-2-naphthyl)-1-pyridin-4-ylprop-2-en-1-one, III, C19H15NO2, the configuration of the keto group is syn with respect to the olefinic double bond. In all three structures the molecules pack with weak intermolecular C–H···O interactions
utilizing both the methoxy and keto oxygen’s in I, the methoxy oxygen in II and the keto oxygen in III. These interactions link the molecules into chains diagonally along the (011) plane of the unit cell in I and III and along the (010) plane in II. The dihedral angle between the phenyl and 2-napthyl rings in I is 31.7(3)°. In II and III the dihedral angle between the pyridyl and 2-naphthyl rings is 14.4(9)° and 1.8(9)°, respectively. C–H···O hydrogen bonding
interactions influence these twist angles of these rings in I–III while weak π–π stacking interactions between naphthyl rings in I and III and also between pyridyl and naphthyl rings in II help stabilize crystal packing. [I: P2
1
/c, a = 7.6635(4) ?, b = 11.8047(6) ?, c = 16.7584(7) ?, β = 99.271(5)°, V = 1496.25(13) ?3; II: Pbca, a = 14.1424(4) ?, b = 6.0957(2) ?, c = 33.1458(11) ?, V = 2857.43(16) ?3; III: P2
1
/c, a = 11.5155(4) ?, b = 6.0020(2) ?, c = 22.4645(8) ?, β = 103.002(4)°, V = 1512.85(9) ?3].
Index Abstract Crystal structures from three Chalcones derived from 6-methoxy-2-naphthaldehyde are reported and their geometric and packing
parameters described. 相似文献
6.
Spring M. Downer Philip J. Squattrito Naima Bestaoui Abraham Clearfield 《Journal of chemical crystallography》2006,36(8):487-501
Salts of 5-aminonaphthalene-2-sulfonate with divalent Mg, Mn, Co, and Ni cations have been crystallized and their structures determined by single crystal X-ray methods. The Mg, Mn, and Co salts are isostructural. Crystal data for hexaaquamagnesium(II) 5-aminonaphthalene-2-sulfonate hexahydrate, [Mg(H2O)6](H2NC10H6SO3)2·6H2O: monoclinic, P21/c, Z=2, a=14.1329(18) ?, b=8.5789(11) ?, c=12.4880(17) ?, β=93.374(3)°, V=1511.5(3) ?3; hexaaquamanganese(II) 5-aminonaphthalene-2-sulfonate hexahydrate, [Mn(H2O)6](H2NC10H6SO3)2·6H2O: monoclinic, P21/c, Z=2, a=14.249(3) ?, b=8.5940(17) ?, c=12.505(3) ?, β=93.30(3)°, V=1528.8(6) ?3; hexaaquacobalt(II) 5-aminonaphthalene-2-sulfonate hexahydrate, [Co(H2O)6](H2NC10H6SO3)2·6H2O: monoclinic, P21/c, Z=2, a=14.1406(18) ?, b=8.5674(11) ?, c=12.4960(16) ?, β=93.297(2)°, V=1511.4(3) ?3. The structures are composed of alternating layers of octahedral metal–aqua complexes and sulfonate anions linked by hydrogen bonds. The three water molecules of crystallization are associated with the hexaaquametal cations and sulfonate O atoms. The repeat unit along the a-axis is a single layer. The Ni salt [crystal data for tetraaquabis(5-aminonaphthalene-2-sulfonato-N)nickel(II) dihydrate, [Ni(H2O)4(H2NC10H6SO3)2]·2H2O: triclinic, , Z=1, a=6.8524(10) ?, b=8.3094(12) ?, c=11.4832(17) ?, α=69.003(2)°, β=76.570(3)°, γ=83.952(2)°, V=593.56(15) ?3] has a very different structure with direct coordination of the amine N atom to Ni, a modified stacking pattern, and fewer free water molecules. Ag and Ni salts of an amine-substituted naphthalenedisulfonate have also been characterized. Crystal data for diaqua(6-ammonionaphthalene-1,3-disulfonato-O)silver(I) hydrate,[Ag(H2O)2(H3NC10H5(SO3)2)]·0.42H2O: monoclinic, P21/c, Z=2, a=9.099(3) ?, b=21.406(6) ?, c=7.629(2) ?, β=110.178(4)°, V=1394.9(7) ?3; tetraaquabis (6-ammonionaphthalene-1,3-disulfonato-O)nickel(II)tetrahydrate, [Ni(H2O)4(H2NC10H5 (SO3)2)2]·4H2O: triclinic,, Z=1, a=6.7971(17) ?, b=10.661(3) ?, c=11.165(3) ?, α=68.308(4)°, β=88.292(5)°, γ=84.896(5)°, V=748.8(3) ?3. The silver salt contains six coordinate metal centers each of which bonds to four sulfonate O atoms from three different anions and two water molecules. The nickel salt contains octahedral cations with four water molecules and two trans sulfonate O atoms. Both structures are layered, but differently from each other and from those of the monofunctional naphthalenesulfonate salts.Unusual coordination of a sulfonate group to a transition metal and coordination of an amine group to nickel but not to cobalt or manganese have been observed in a series of metal aminonaphthalenesulfonate salts 相似文献
7.
L. B. Serezhkina E. V. Peresypkina A. V. Virovets A. G. Verevkin D. V. Pushkin 《Crystallography Reports》2009,54(2):259-266
Single crystals of the compounds (C3N6 H7)4(CN3H6)2[UO2(CrO4)4] · 4H2O (I) and (H3O)6[UO2(CrO4)4] (II) are synthesized, and their structures are investigated using X-ray diffraction. Compound I crystallizes in the triclinic system with the unit cell parameters a = 6.3951(8) ?, b = 10.8187(16) ?, c = 16.9709(18) ?, α = 93.674(4)°, β = 97.127(4)°, γ = 92.020(4)°, space group, P
Z = 1, V = 1161.6(3) ?3, and R = 0.0470. Crystals of compound II belong to the monoclinic system with the unit cell parameters a = 14.3158(4) ?, b = 11.7477(3) ?, c = 13.1351(4) ?, β= 105.836(1)°, space group C2/c, Z = 4, V = 2125.2(1) ?3, and R = 0.0213. The uranium-containing structural units of crystals I and II are mononuclear anionic complexes of the composition [UO2(CrO4)4]6− with an island structure, which belong to the crystal-chemical group Am
14 (A = UO2+2, M
1 = CrO2−4) of the uranyl complexes. The [UO2(CrO4)4]6− anionic complexes are joined into a three-dimensional framework through the electrostatic interactions with outer-sphere
cations and a system of hydrogen bonds.
Original Russian Text ? L.B. Serezhkina, E.V. Peresypkina, A.V. Virovets, A.G. Verevkin, D.V. Pushkin, 2009, published in
Kristallografiya, 2009, Vol. 54, No. 2, pp. 284–290. 相似文献
8.
L. B. Serezhkina M. S. Grigor’ev I. S. Kuz’menko V. N. Serezhkin 《Crystallography Reports》2012,57(2):258-263
Compounds K2[UO2(C3H2O4)2] · H2O (I) and Rb2[UO2(C3H2O4)2] · H2O (II) are synthesized and their crystal structures are determined by X-ray diffraction. The compounds crystallize in the monoclinic
crystal system; for I, a = 7.1700(2) ?, b =12.3061(3) ?, c = 14.3080(4) ?, β = 95.831(2)°, space group P21/n, Z = 4, and R = 0.0275; for II, a = 7.1197(2) ?, b = 12.6433(4) ?, c = 14.6729(6) ?, β = 96.353(2)°, space group P21/n, Z = 4, and R = 0.0328. It is found that I and II are isostructural. The main structural units of the crystals are the [UO2(C3H2O4)2]2− chains, which belong to the AT
11
B
01 (A = UO22+, T
11, and B
01 = C3H2O42−) crystal chemical group of uranyl complexes. The chains and alkali metal ions R (R = K or Rb) are connected by electrostatic interactions and hydrogen bonds. Some specific structural features of [UO2(C3H2O4)2]2− complex groups are discussed. 相似文献
9.
Mario V. Capparelli Jaime E. Charris José N. Domínguez 《Journal of chemical crystallography》2006,36(6):389-398
The crystal structures of two N-methylated tricyclic quinolones were determined. 3-amino-6-methoxy-9-methyl-(1H)pyrazolo[3,4-b]-4-quinolone hydrate, C12H12N4O2 · H2O (1) crystallizes in P-1 with a=11.5078(18) ?, b=13.0614(19) ?, c=9.0860(15) ?, α=106.229(4)°, β=108.378(3)°, γ=71.118(3)° and Z=4, while 2,4-diamino-10-methyl-9-methoxypyrimido[4,5-b]-5-quinolone, C13H13N5O2 (2) crystallizes in P21/n with a=10.6643(17) ?, b=10.1114(17) ?, c=11.3185(18) ?, β=99.351(4)° and Z=4. Both molecules are essentially planar, including the exocyclic groups. 1 and 2 have moderate antimalarial activity which seems to be related to the formation of intramolecular N – H · · · O=C hydrogen bonds; 1 does not form these bonds and has approximately twice the activity of 2. In both crystal structures there are extensive networks of N–H · · · O and N–H · · · N hydrogen bonds, and in 1 the water molecules of solvation form N–H · · · Ow, Ow–H · · · O=C and Ow–H · · · Ow bonds. 相似文献
10.
Gang Wu Yan Wang Xiao-Feng Wang Hiroyuki Kawaguchi Wei-Yin Sun 《Journal of chemical crystallography》2007,37(3):199-205
Two complexes (H2bipy)[M2(TB)2(H2O)8]·5H2O (M = Mn 1, Zn 2) (bipy = 4,4′-bipyridine, H3TB = 1,3,5-tris(carboxymethoxyl)benzene) were synthesized by the reaction of the corresponding metal salt with ligand H3TB and 4,4′-bipy in an aqueous methanol solution at room temperature, respectively. Their structures were determined by single
crystal X-ray diffraction analysis. Both complexes 1 and 2 crystallize in the triclinic space group with the crystal parameters of 1: a = 9.725(12) ?, b = 10.651(13) ?, c = 10.882(13) ?, α = 91.72(2)°, β = 96.41(2)°, γ = 97.72(2)°, V = 1109(2) ?3, Z = 1 and 2: a = 9.610(10) ?, b = 10.55(2) ?, c = 10.83(2) ?, α = 91.60(4)°, β = 95.32(2)°, γ = 97.73(4)°, V = 1082(3) ?3, Z = 1. Complexes 1 and 2 have the same dinuclear structure, in which each metal atom is six coordinated with distorted octahedral geometry by two
oxygen atoms from two different TB3− ligands and four ones from four coordinated water molecules. The dinuclear units are further linked by hydrogen bonding and
π–π interactions to form the three-dimensional framework structure. 相似文献
11.
R. Alan Howie Marcus V. N. de Souza Camilo H. da Silva Lima James L. Wardell Solange M. S. V. Wardell 《Journal of chemical crystallography》2012,42(4):394-400
Abstract
The molecule of (E)-3-(3-MeOC6H4CH=CHCO)-benzotriazole 1-oxide, 2, has a very near planar structure, while the 2-nitrophenyl ring is rotated out of the plane of the remaining atoms in (E)-3-(2-O2NC6H4CH=CHCO)-benzotriazole 1-oxide, 1. The nitrogen oxide bond lengths in 1 and 2 are 1.258 (6) and 1.2683 (15) ?, respectively, and are in the region found for related compounds. There are no strong intermolecular hydrogen-bonds in either compound, instead there are weak C–H···O intermolecular hydrogen-bonds and π···π stacking interactions in 1, and C–H···O, C–H···π, and π···π stacking interactions in 2. Different three-dimensional arrays are generated in each case. Compound 1 crystallises in the orthorhombic space group Pna21, with a = 25.061 (2) ?, b = 3.6997 (2) ?, c = 14.2623 (12) ? and Z = 4. Compound 2 crystallises in the triclinic space group P-1, with a = 5.7297 (3) ?, b = 10.8440 (6) ?, c = 11.4965 (6) ?, α = 89.689 (3)°, β = 76.019 (3)°, γ = 75.047 (3)°, Z = 2. 相似文献12.
Ying Liu Jianmin Dou Daqi Wang Dacheng Li Zhaoping Gao 《Journal of chemical crystallography》2006,36(10):613-618
Two new transition metal complexes of [M(OH2)(HDPA)2]·3H2O (M=Mn(1); M=Co(2)) (H2DPA, 2,6-pyridine-dicarboxylic acid) have been prepared at room temperature from the reaction of MCl2·6H2O (M=Mn or Co) and H2DPA in the mixed solvent of H2O and EtOH in the presence of piperazine, and were characterized by X-ray analysis, elemental analysis. X-ray analysis reveals that the coordination geometries of Mn2+ and Co2+ are of octahedron and severely distorted square-based pyramid, respectively. Crystal data: [Mn(OH2)(HDPA)2]·3H2O (1), Mr=459.23, monoclinic, P2(1)/n, a=7.0056(3), b=(23.8125(12), c=10.7444(3) ?, β=99.834(2)°, Z=4, V=1766.28(13) ?3, R
1=0.0586, wR
2=0.1448 [I>2σ(I)]; Co(OH2)(HDPA)2]·3H2O (2), Mr=463.22, monoclinic, P2(1)/n, a=7.0014(2), b=23.8346(7), c=10.7212(4) ?, β=99.8540(10)°, Z=4, V=1762.71(10) ?3, R
1=0.0474, wR
2=0.1366 [I>2σ(I)]. 相似文献
13.
Abstract
Two new complexes [Ni(tren)(pic)]2(ClO4)2·CH3OH (1) and [Co(tren)(dipic)]ClO4·CH3OH (2), (tren is tris(2-aminoethyl)amine, pic is the anion of picolinic acid, dipic is the dianion of 2,6-pyridinedicarboxylic acid) have been synthesized and structurally characterized. X-ray analysis indicates that the two complexes are mononuclear with tren acting as a quadridentate ligand. In complex 1, the nickel(II) ion is further coordinated with picolinate in μ2-N, O bidentate chelating mode. In complex 2, the cobalt(III) ion is coordinated with the pyridine nitrogen and one carboxylic oxygen of 2,6-pyridinedicarboxylate in μ2-N, O chelating form. The metal atoms in both cases have distorted octahedral geometry. Crystal data: [Ni(tren)(pic)]2(ClO4)2·CH3OH (1), Mr = 869.03, monoclinic, C2/c, a = 26.354(5) ?, b = 10.407(2) ?, c = 25.839(5) ?, β = 96.24(3)°, Z = 8, V = 7045(2) ?3, R 1 = 0.0418, wR 2 = 0.1063 [I > 2σ(I)]; [Co(tren)(dipic)]ClO4·CH3OH (2), Mr = 501.77, Triclinic, P-1, a = 8.3667(2) ?, b = 10.4434(2) ?, c = 11.9431(16) ?, α = 73.9590(10)°, β = 88.0240(10)°, γ = 75.5890°, Z = 2, V = 969.97(4) ?3, R 1 = 0.0408, wR 2 = 0.1063 [I > 2σ(I)]. 相似文献14.
Octavio A. C. Antunes Jairo Bordinhão Nakédia M. F. Carvalho James L. Wardell Pedro A. Arroyo Márcio E. Berezuk Lucio Cardozo-Filho Edward R. T. Tiekink 《Journal of chemical crystallography》2007,37(4):291-298
Two structures of the closely related piperazinium salts, [1,4-bis-(2-methoxy-2-carbonylethyl)piperazinium (2+)] chloride
(1) and [1,4-bis-(2-amidoethyl)piperazinium (2+)] perchlorate (2) reveal the persistence of a layer structure, interspersed with anions, held in place by N–H···Cl, C–H···O and C–H···Cl interactions
in the case of 1, and N–H···O and C–H···O interactions in the case of 2. Compound 1 crystallizes in the triclinic space group P-1 with a=6.7667(6) ?, b = 6.9467(6) ?, c=9.3880(18) ?, α=105.845(9)°, β=99.896(16)°, γ=103.600(9)°, and Z=1. Compound 2 crystallizes in the monoclinic space group P21/c with a = 9.0930(8) ?, b=10.0525(11) ? c=10.2104(13) ?, β=114.279(9)°, and Z=2. 相似文献
15.
Manjit K. Bhattacharyya Sanchay J. Bora Birinchi K. Das 《Journal of chemical crystallography》2008,38(3):195-203
Abstract A new complex containing two different substituted pyridine ligands, viz. 4-CNpy (4-cyanopyridine) and pdc (pyridine-2,6-dicarboxylate),
[Ni(H2O)2(pdc)(4-CNpy)] · 2H2O (1), has been prepared using [Ni(4-CNpy)2(H2O)3(SO4)] · H2O (2) as the starting compound. Crystal data on 1 are: monoclinic, P21/c, a = 11.533(2) ?, b = 20.114(4) ?, c = 7.306(1) ?, β = 93.777(3)°, V = 1,691.1(5) ?3, Z = 2, D
calc. = 1.57 g cm−3, R
1 = 0.0585, w R
2 = 0.1236 for reflections with I > 4σ(F
0) and 268 parameters (R
1 = 0.0859, wR
2 = 0.1336 for all 4,024 reflections). The discrete molecules of the title complex remain hydrogen-bonded to assemble into
supramolecular layers interleaved by disordered water molecules. In an attempt to obtain the cationic complex species cis-[Ni(H2O)4(4-CNpy)2]2+ we have isolated the compound [Ni(H2O)4(4-CNpy)2] · (BPh4)2 · 2(4-CNpy) · 4H2O (3) by adding NaBPh4 to an aqueous solution of 2. Crystal data on 3 are: monoclinic, P21/n, a = 10.5002(1) ?, b = 21.1692(3) ?, c = 15.3249(2) ?, β = 95.120(1)°, V = 3392.84(7) ?3, Z = 2, D
calc. = 1.231 g cm−3, R
1 = 0.0453, wR
2 = 0.1217 for reflections with I > 4σ (F
0) and 556 parameters (R
1 = 0.0688, wR
2 = 0.1364 for all 9,257 reflections).
Index Abstract Synthesis and Crystal Structure of [Ni(H2O)2(pdc)(4-CNpy)] · 2H2O (pdc = Pyridine-2,6-dicarboxylate, 4-CNpy = 4-cyanopyridine)
Manjit K. Bhattacharyya, Sanchay J. Bora and Birinchi K. Das
Crystal structure of a new nickel(II) complex displaying a supramolecular layered structure is described.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
16.
Xiang-Shan Wang Zhao-Sen Zeng Da-Qing Shi Shu-Jiang Tu Xian-Yong Wei Zhi-Min Zong 《Journal of chemical crystallography》2006,36(11):697-701
The crystal structure of 2-amino-3-cyano-4,6-dihydro-4-(3-nitrophenyl)-5H-pyrano[3,2-c]quinolin-5-one N,N-dimethylformamide solvate monohydrate is determined by room temperature X-ray diffraction. The title compound 1, C22H21N5O6, is triclinic, space group P-1, a=9.109(2) ?, b=11.340(2) ?, c=12.485(2) ?, α=70.02(1)°, β=69.36(1)°, γ=67.32(1)°, Z=2, V=1081.4(4) ?3. It is interesting that a bridge-like hydrogen bond O–H···O is formed between the title compound and solvent molecules of water with molecular ratio of 2:2 building a bi-layer framework. In addition, there are two other types of classical hydrogen bonds N–H···N and N–H···O in the crystal structure.Supplementary material Crystallographic data for the structure reported in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publication no. CCDC-275001. Copies of available material can be obtained, free of charge, on application to the Director, CCDC, 12 Union Road, Cambridge CB2 1EZ, UK, (fax: +44-(0) 1223–336033 or e-mail: deposit@ccdc.cam.ac.uk). 相似文献
17.
Abstract
Two phosphate salts (2-aminopyrimidine): (phosphoric acid): H2O [HL1+ (H2PO4) − ]·H2O (1), and (4-phenylthiazol-2-amine): (phosphoric acid) [HL2+·(H2PO4)−] (2) based on 2-aminoheterocyclic compounds, 2-aminopyrimidine (L1), and 4-phenylthiazol-2-amine (L2) were prepared and structurally characterized by X-ray crystallography. Compound 1 crystallizes in the triclinic, space group P-1, with a = 6.2201(7) Å, b = 8.6139(9) Å, c = 9.4800(10) Å, α = 109.685(2)°, β = 106.3340(10)°, γ = 95.4450(10)°, V = 448.72(8) Å3, Z = 2. For 1, the cations were linked to each other via intermolecular C–H···N hydrogen bonds to form a 1-D chain structure running along the a-axis direction. The anions and the water molecules were connected alternatively along the a-axis direction through O–H···O hydrogen bonds to form a 1-D chain also. The cationic chains and the anionic chains were alternatively connected along the c-axis direction through N–H···O and C–H···O hydrogen bonds to form a 2D corrugated sheet. Adjacent sheets were combined together through π–π interaction to form double sheet. These double sheets were further joined together by O–H···O and N–H···O hydrogen bonds to produce a 3D network structure. Compound 2 crystallizes in the Orthorhombic, space group Pbca, with a = 10.1929(10) Å, b = 8.4406(9) Å, c = 27.589(2) Å, α = 90°, β = 90°, γ = 90°, V = 2373.6(4) Å3, Z = 8. In 2, the phosphates formed 1D chain along the b-axis through two P–O–H···O = P hydrogen bonds. The cations formed 1D zigzag chain along the b-axis direction under the CH–π interaction. The anionic chains were intercalated between two adjacent cationic chains through N–H···O, O–H···O, C–H···O, and O–S contacts. Such stacking repeated along the c-axis direction to form a 3D network structure. 相似文献18.
Ying Liu Jianmin Dou Daqi Wang Xianxi Zhang Dacheng Li Yingchun Jia 《Journal of chemical crystallography》2011,41(2):186-191
Abstract
The novel dimeric manganese-substituted polyoxotungstate Na10[(α-B-ZnW9O34)2W2Mn2(H2O)2](OH)2·34H2O (1) has been designed and synthesized from the hydrothermal reaction of Na2WO4·2H2O, MnCl2·4H2O, and ZnCl2 in a Teflon-lined stainless steel autoclave at 140°. X-ray diffraction analysis results reveal that compound (1) crystallizes in the monoclinic system, space group P2(1)/n, with a = 13.0901(3) ?, b = 17.8242(4) ?, c = 21.2401(5) ?, β = 93.6380(10)°, Z = 1, V = 4945.8(2) ?3, F(000) = 5244, Dc = 3.974 g/cm−3, μ(Mo-Kα) = 2.4037 cm−1, λ(Mo-Kα) = 0.71073 ?. The structure was refined to R = 0.0631 and wR = 0.1532. The polyoxoanion of [(α-B-ZnW9O34)2W2Mn2(H2O)2]8− consist of two Keggin lacunary α-B-ZnW9O34 12− moieties linked via a rhomblike W2Mn2O16 group leading to a sandwich-type structure. 相似文献19.
Hai-Yun Zhu 《Journal of chemical crystallography》2011,41(11):1785-1789
Abstract
Two new hydrazone compounds, 3-bromo-N′-(2-methoxybenzylidene)benzohydrazide (1) and N′-(2-methoxybenzylidene)-3,4-methylenedioxybenzohydrazide (2), have been synthesized and characterized by elemental analysis, IR, and single crystal X-ray diffractions. Compound (1) crystallizes in the triclinic space group P1 with unit cell dimensions a = 8.4088(5) ?, b = 8.5398(5) ?, c = 10.6572(6) ?, α = 90.356(3)°, β = 102.868(3)°, γ = 97.987(3)°, V = 738.28(7) Ǻ3, Z = 2, R 1 = 0.0406, and wR 2 = 0.0804. Compound (2) crystallizes in the tetragonal space group P41 with unit cell dimensions a = b = 9.792(4) ?, c = 15.788(6) ?, V = 1513.8(10) Ǻ3, Z = 4, R 1 = 0.0415, and wR 2 = 0.0818. The molecules of both compounds display E configurations with respect to the C=N double bonds. In the crystal structure of (1), molecules are linked through N–H···O hydrogen bonds, forming chains running along the b axis. In the crystal structure of (2), molecules are linked through N–H···O hydrogen bonds, forming chains running along the c axis. 相似文献20.
Abstract A pair of CuII coordination isomers [Cu(pmt)2] · 4H2O (1) and {[Cu(pmt)2] · 2H2O}
n
(2) [Hpmt = 2-(2-pyridylmethylamino) ethanesulfonic acid] have been prepared by reaction of the same proportion CuCl2 · 2H2O and Hpmt but with different experimental methods in water–methanol mixed solution, and were characterized by X-ray diffraction,
elemental analysis, IR spectrum. X-ray analysis indicates that complex (1) is a mononuclear complex in which two deprotonated pmt ligands coordinate in a facial tridentate arrangement about the CuII atom. While complex (2) is a coordination polymer, in which four N atoms of pmt ligands coordinate to one CuII atom but its sulfonate O atoms bond to adjacent CuII atom. Thus 12-membered rings (–Cu–N–C–C–S–O–)2 are obtained between two neighbouring CuII atoms and they connect one another to form this new polymer. Crystal data: [Cu(pmt)2] · 4H2O (1), Mr = 566.10, monoclinic, P2
1/c, a = 9.1950(8) ?, b = 11.5093(10) ?, c = 11.2304(10) ?, β = 105.5550(10)°, Z = 2, V = 1144.96(17) ?3, R
1
= 0.0407, wR
2
= 0.1242 [I > 2σ (I)]; {[Cu(pmt)2] · 2H2O}
n
(2), Mr = 530.07, triclinic, P-1, a = 7.6165(19) ?, b = 8.806(2) ?, c = 9.592(4) ?, α = 104.933(4)°, β = 106.732(4)°, γ = 109.503(3)°, Z = 1, V = 534.2(3) ?3, R
1 = 0.0470, wR
2 = 0.1082 [I > 2σ(I)].
Index Abstract A pair of CuII coordination isomers [Cu(pmt)2] · 4H2O (1) and {[Cu(pmt)2] · 2H2O}
n
(2) [Hpmt = 2-(2-pyridylmethylamino) ethanesulfonic acid] have been prepared by reaction of the same proportion CuCl2 · 2H2O and Hpmt but with different experimental methods in water–methanol mixed solution.
相似文献