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1.
Karen A. Ketcham Isabel Garcia Elena Bermejo John K. Swearingen Alfonso Castieiras Douglas X. West 《无机化学与普通化学杂志》2002,628(2):409-415
Reduction of 2‐cyanopyridine by sodium in the presence of 3‐hexamethyleneiminylthiosemicarbazide produces 2‐pyridineformamide 3‐hexamethyleneiminylthiosemicarbazone, HAmhexim. Complexes with nickel(II), copper(II) and palladium(II) have been prepared and the following complexes structurally characterized: [Ni(Amhexim)OAc], [{Cu(Amhexim)}2C4H4O4]·2DMSO·H2O, [Cu(HAmhexim)Cl2] and [Pd(Amhexim)Cl]. Coordination is via the pyridyl nitrogen, imine nitrogen and thiolato or thione sulfur atom when coordinating as the anionic or neutral ligand, respectively. [{Cu(Amhexim)}2C4H4O4] is a binuclear complex with the two copper(II) ions bridged by the succinato group in [Cu‐(HAmhexim)Cl2] the Cu atom is 5‐coordinate and close to a square pyramid structure and in [Ni(Amhexim)OAc] and [Pd(Amhexim)Cl] the metal atoms are planar, 4‐coordinate. 相似文献
2.
Elena Bermejo Alfonso Castieiras Lily J. Ackerman Matthew D. Owens Douglas X. West 《无机化学与普通化学杂志》2001,627(8):1966-1971
The crystal structure of a copper(II) complex of 2‐acetylpyridine 3‐piperidylthiosemicarbazone, [Cu(Acpip)2], indicates a tridentate, monoanionic ligand (i. e., pyridine nitrogen, imine nitrogen and thiolato sulfur atoms) and a bidentate, monanionic ligand (i. e., imine nitrogen and thiolato sulfur atoms). The stereochemistry approaches square pyramidal with the bidentate ligand occupying an apical (imine nitrogen atom) and basal (thiolato sulfur atom) position. The structure of a nickel(II) complex of 1‐phenylglyoxal N(4)‐diethylthiosemicarbazone, [Ni(Pg4DE)], has a 4‐6‐5 trichelate system rather than the 5‐5‐5 system common to bis(thiosemicarbazones). Coordination of the hydrazinic nitrogen atom of the “phenyl arm” along with the thiolato sulfur atom provides the 4‐membered chelate ring. 相似文献
3.
Jerry P. Jasinski Jason R. Bianchani Juan Cueva Fathy A. El‐Saied Ahmed A. El‐Asmy Douglas X. West 《无机化学与普通化学杂志》2003,629(2):202-206
Copper(II) complexes of 3, 4‐hexanedione bis(piperidyl‐ and bis(hexamethyleneiminylthiosemicarbazone), H2Hxpip and H2Hxhexim, respectively, have been prepared and studied spectroscopically. The bis(thiosemicarbazones) have been characterized by their melting points, as well as IR, electronic and 1H NMR spectra. Upon formation of their copper(II) complexes, loss of the hydrazinic hydrogen atoms occurs, and the ligands coordinate as dianionic, tetradentate N2S2 ligands. The crystal structures of H2Hxpip, its 4‐coordinate copper(II) complex, [Cu(Hxpip)], and the related [Cu(Hxhexim)] have been determined by single crystal x‐ray diffraction. The nature of the four‐coordinate copper(II) complexes have also been characterized by ESR, IR, and electronic spectroscopy, as well as magnetic moments and elemental analyses. 相似文献
4.
Elena Bermejo Alfonso Castieiras Isabel García‐Santos Douglas X. West 《无机化学与普通化学杂志》2004,630(7):1096-1109
Sodium in dry methanol reduces 2‐cyanopyridine in the presence of 3‐hexamethyleneiminylthiosemicarbazide and produces 2‐pyridineformamide 3‐hexamethyleneiminylthiosemicarbazone, HAmhexim ( 1 ). Complexes with zinc(II ), cadmium(II ) and mercury(II ) have been prepared and characterized by spectroscopic techniques. In addition, the crystal structures of HAmhexim ( 1 ), [Zn(Amhexim)(OAc)]2μ·μDMSO ( 2 ), [Cd(HAmhexim)Cl2]μ·μDMSO ( 7 ), [Cd(Amhexim)2] ( 8 ), [Cd(HAmhexim)Br2]μ·μDMSO ( 9 ), [Cd(HAmhexim)I2]μ·μEtOH ( 10 ), [Hg(HAmhexim)Cl2]μ·μDMSO ( 11 ), [Hg(Amhexim)Br]2 ( 13 ), [Hg3(HAmhexim)(Amhexim)Br5]μ·μH2O ( 14 ) and [Hg(Amhexim)I]2 ( 15 ) have been determined. Coordination of the anionic and neutral thiosemicarbazone ligand occurs through the pyridine nitrogen atom, imine nitrogen atom, and thiolato or thione sulfur atom. In [Zn(Amhexim)(OAc)]2 one of the bridging acetato ligands has monodentate coordination and the other bridges in a bidentate manner. [Cd(Amhexim)2] is a 6‐coordinate species while the other cadmium complexes are 5‐coordinate. In [Hg(Amhexim)Br]2 and [Hg(Amhexim)I]2 the thiolato sulfur atoms act as bridges between the Hg atoms to form dimeric compounds and [Hg3(HAmhexim)(Amhexim)Br5]μ·μH2O is a trinuclear complex with three different centers — two metallic centers have a 5‐coordination and the another one has 4‐coordination. In addition, [Hg(HAmhexim)Cl2]μ·μDMSO and [Hg3(HAmhexim)(Amhexim)Br5]μ·μH2O shown a supramolecular one‐dimensional hydrogen‐bonded self‐assembling. 相似文献
5.
Jos S. Casas Alfonso Castieiras Emilia García‐Martínez Yolanda Paraj M. Luz Prez‐Parall Angeles Snchez‐Gonzlez Jos Sordo 《无机化学与普通化学杂志》2005,631(11):2258-2264
Compounds of type [MX2(Hpben)] [M = Pd (X = Cl), Pt (X = Cl, I); Hpben = 2‐(2′‐pyridyl)benzimidazole] were prepared and characterized, and the structures of the Pt derivatives were determined by X‐ray crystallography. The crystals of [PtI2(Hpben)] consist of discrete units in which the Pt atom is coordinated to two iodine atoms and to pyridine and imidazole N atoms in a distorted square planar arrangement. The structure of the chloro derivative is similar, except that the [PtCl2(Hpben)] monomers are hydrogen‐bonded in zig‐zag chains. In assays of the interactions of the Pd and Pt chloro compounds with DNA, and of their in vitro cytotoxic activity against human cervical carcinoma cells (HeLa‐229), human ovarian carcinoma cells (A2780) and a cisplatin‐resistant mutant A2780 line (A2780cis), the only activity observed was modest cytotoxicity of the Pd derivative for A2780. 相似文献
6.
Jun‐Feng Zhang Xin Gan Quan‐Qing Xu Jian‐Hua Chen Mei Yuan Wen‐Fu Fu Prof. Dr. 《无机化学与普通化学杂志》2007,633(10):1718-1722
The reactions of pyrimidine‐phosphine ligand N‐[(diphenylphosphino)methyl]‐2‐pyrimidinamine ( L ) with various metal salts of PtII, PdII and CuI provide three new halide metal complexes, Pt2Cl4(μ‐L)2·2CH2Cl2 ( 1 ), Pd2Cl4(μ‐L)2 ( 2 ), and [Cu2(μ‐I)2L2]n ( 3 ). Single crystal X‐ray diffraction studies show that complexes 1 and 2 display a similar bimetallic twelve‐membered ring structure, while complex 3 consists of one‐dimensional polymeric chains, which are further connected into a 2‐D supramolecular framework through hydrogen bonds. In the binuclear complexes 1 and 2 , the ligand L serves as a bridge with the N and P as coordination atoms, but in the polymeric complex 3 , both bridging and chelating modes are adopted by the ligand. The spectroscopic properties of complexes 1 ‐ 3 as well as L have been investigated, in which complex 3 exhibits intense photoluminescence originating from intraligand charge transfer (ILCT) π→π* and metal‐to‐ligand charge‐transfer (MLCT) excited states both in acetonitrile solution and solid state, respectively. 相似文献
7.
Elena Bermejo Alfonso Castieiras Maria Gil Elena Labisbal Antonio Sousa Heloisa Beraldo Douglas X. West 《无机化学与普通化学杂志》2001,627(5):827-835
Pyridil bis(N(4)‐substituted thiosemicarbazones) have been prepared in which the substituents in place of the NH2 group in the thiosemicarbazone moieties are piperidinyl (H2Plpip), hexamethyleneiminyl (H2Plhexim), diethylaminyl (H2Pl4DE), and dipropylaminyl (H2Pl4DP). IR, electronic, mass, and ESR spectra of their copper(II) complexes are reported. Crystal structure determinations of H2Pl4DE and three of the copper(II) complexes of formula [Cu(Plpip)], [Cu(Plhexim)] and [Cu(Pl4DE)]2 · 2[Cu(Pl4DE)], are included. H2Pl4DE lacks hydrogen bonding between the thiosemicarbazone moieties, but each moiety is in the Z configuration form with hydrogen bonding from the thiosemicarbazone moieties to the pyridyl nitrogen atoms. The crystal used for the structure determination of [Cu(Plhexim)] was isolated from an electrochemical preparation. In all the new compounds the deprotonated ligands are N,N,S,S‐tetradentate, coordinating to the copper(II) centre through their azomethine nitrogen atoms and their thiocarbonyl sulfur atoms. 相似文献
8.
Mohammad Yazdanbakhsh Mohammad Hakimi Majid M. Heravi Mitra Ghassemzadeh Bernhard Neumüller 《无机化学与普通化学杂志》2004,630(5):627-629
The reaction of 4‐amino‐1, 2, 4‐triazin‐3(2H)‐thione‐5‐one (ATTO, 1 ) with [Cu(PPh3)2]NO3 in ethanol led to the complex [Cu(PPh3)2(ATTO)]NO3 ( 2 ). 2 was characterized by elemental analyses, IR, 1H NMR and Raman spectroscopy. A single‐crystal X‐ray diffraction of compound 2 revealed that ATTO acts as a bidentate ligand via its nitrogen and sulfur atoms. Crystal data for 2 at 20 °C: space group P21/n with a = 975.7(1), b = 1533.5(2), c = 2504.2(3) pm, β = 92.25(1)°, Z = 4, R1 = 0.0632. 相似文献
9.
Maria Gil Elena Bermejo Alfonso Castieiras Heloisa Beraldo Douglas X. West 《无机化学与普通化学杂志》2000,626(11):2353-2360
Pyridyl bis(N(4)‐substituted thiosemicarbazones), in which the substituents replacing the NH2 group on the thiosemicarbazone moieties are piperidyl, H2Plpip; hexamethyleneiminyl, H2Plhexim; diethylamino, H2Pl4DE; and dipropylamino, H2Pl4DP, have been synthesized. These bis(thiosemicarbazones) and their nickel(II) complexes have been characterized with IR, electronic, mass, and 1H and 13C NMR spectra. Crystal structures have been solved for H2Plpip and all four nickel(II) complexes. H2Plpip does not possess hydrogen bonding between the thiosemicarbazone moieties, but is in the Z isomeric form with intramolecular hydrogen bonding from both thiosemicarbazone moieties to pyridine nitrogen atoms. The nickel(II) complexes possess square‐planar N2S2 (i. e., imine nitrogen and thiolato sulfur atoms) centers and the two pyridine ring nitrogen atoms are not coordinated. 相似文献
10.
Luca Rigamonti Stefano Carlino Carlo Castellano Prof. Dr. Francesco Demartin Prof. Dr. Alessandro Pasini 《无机化学与普通化学杂志》2012,638(14):2252-2256
The X‐ray structures of 4‐amidiniumpyridine acetate, ( 1· H)AcO, and of cis‐[Pt( 1 )2(PPh3)2](NO3)2 ( 2 ), as well as their IR spectra, reveal intramolecular hydrogen bonding, which held together the cations and the anions. The IR spectroscopic data suggest that this may be so also in cis‐[PtCl( 1 )(PPh3)2](BF4) ( 3 ). In ( 1· H)AcO and in 2 extensive intermolecular hydrogen bonding networks span through the whole crystals. 相似文献
11.
Jesús Martínez Rufina Bastida Alejandro Macías Laura Valencia Manuel Vicente 《无机化学与普通化学杂志》2005,631(11):2046-2053
The pendant‐armed ligands L1 and L2 were synthesized by N‐alkylation of the four secondary amine groups of the macrocyclic precursor L using o‐nitrobenzylbromide (L1) and p‐nitrobenzylbromide (L2). Nitrates and perchlorates of CuII, NiII and CoII were used to synthesize the metal complexes of both ligands and the complexes were characterized by microanalysis, MS‐FAB, conductivity measurements, IR and UV‐Vis spectroscopy and magnetic studies. The crystal structures of L1, [CuL1](ClO4)2·CH3CN·H2O, [CuL2](ClO4)2·6CH3CN, [CuL2][Cu(NO3)4]·5CH3CN·0.5CH3OH and [NiL2](ClO4)2·3CH3CN·H2O were determined by single crystal X‐ray crystallography. These structural analysis reveal the free ligand L1, three mononuclear endomacrocyclic complexes {[CuL1](ClO4)2·CH3CN·H2O, [CuL2](ClO4)2·6CH3CN and [NiL2](ClO4)2·3CH3CN·H2O} and one binuclear complex {[CuL2][Cu(NO3)4]·5CH3CN·0.5CH3OH} in which one of the metals is in the macrocyclic framework and the other metal is outside the ligand cavity and coordinated to four nitrate ions. 相似文献
12.
Wolfgang Beck Wolf Peter Fehlhammer Klaus Feldl Thomas M. Klaptke Gernot Kramer Peter Mayer Holger Piotrowski Peter Pllmann Walter Ponikwar Thomas Schütt Erich Schuierer Martin Vogt 《无机化学与普通化学杂志》2001,627(8):1751-1758
The crystal structures of the monomeric palladium(II) azide complexes of the type L2Pd(N3)2 (L = PPh3 ( 1 ), AsPh3 ( 2 ), and 2‐chloropyridine ( 3 )), the dimeric [(AsPh4)2][Pd2(N3)4Cl2] ( 4 ), the homoleptic azido palladate [(PNP)2][Pd(N3)4] ( 5 ) and the homoleptic azido platinates [(AsPh4)2][Pt(N3)4] · 2 H2O ( 6 ) and [(AsPh4)2][Pt(N3)6] ( 7 ) were determined by X‐ray diffraction at single crystals. 1 and 2 are isotypic and crystallize in the triclinic space group P1. 1 , 2 and 3 show terminal azide ligands in trans position. In 4 the [Pd2(N3)4Cl2]2– anions show end‐on bridging azide groups as well as terminal chlorine atoms and azide ligands. The anions in 5 and 6 show azide ligands in equal positions with almost local C4h symmetry at the platinum and palladium atom respectively. The metal atoms show a planar surrounding. The [Pt(N3)6]2– anions in 7 are centrosymmetric (idealized S6 symmetry) with an octahedral surrounding of six nitrogen atoms at the platinum centers. 相似文献
13.
Alfonso Castieiras Ricardo Domínguez Lourdes Gmez‐Rodríguez Joaquín Borrs 《无机化学与普通化学杂志》2003,629(6):1096-1103
A copper(II) and two nickel(II) dinuclear oxalato‐bridged compounds of formulae [{Cu(bpdto)}2(μ‐ox)](ClO4)2 ( 1 ), [{Ni(bpdto)]2(μ‐ox)](ClO4)2( 2 ), and [{Ni(bpdto)}2(μ‐ox)](NO3)2·2H2O ( 3 ), where bpdto = 1, 8‐bis(2‐pyridyl)‐3, 6‐dithiaoctane and ox = oxalate = C2O42— anion, have been synthesized and characterized. The crystal structure of 3 was determined by single‐crystal X‐ray analysis. It is a dinuclear complex with i symmetry in which the oxalate ligand is coordinated in bis(didentate) fashion to the inversion centre‐related nickel atoms. The distorted octahedral environment of each nickel atom is completed by two sulphur atoms in the equatorial plane and by two pyridyl nitrogen atoms in axial positions. Magnetic susceptibility measurements over the range 5 — 299K, show antiferromagnetic interactions that are weak in 1 (J = —12.8 cm—1) and strong in 2 and 3 (J = —37.8 and —40.9 cm—1, respectively), which in the case of 3 is in keeping with the observed structural parameters. 相似文献
14.
Synthesis,Spectral Characterization and Antimicrobial Activity of Some Transition Metal Complexes of 1,3‐Bis(1H‐benzimidazol‐2‐yl)‐2‐oxapropane
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Aydin Tavman Adem Çinarli Demet Gürbüz A. Seher Birteksöz Tan M. A. Faruk Öksüzömer Mayram Tüysüz Mehmet Ali Gürkaynak Bahattin Yalçin 《中国化学会会志》2014,61(12):1377-1387
1,3‐Bis(1H‐benzimidazol‐2‐yl)‐2‐oxapropane ( L ) complexes with Fe(NO3)3, CoCl2, Co(NO3)2, Ni(NO3)2, CuCl2, Cu(ClO4)2, PdCl2, CdI2, Hg(NO3)2 were synthesized and characterized by elemental analysis, molar conductivity, magnetic moment, TGA, FT‐IR, NMR, ESI‐MS, fluorescence spectroscopy. Also, the crystal structure of 1,3‐bis(1H‐benzimidazol‐2‐yl)‐2‐oxapropane]dichlorocobalt(II), [Co( L )Cl2], complex is reported that it has distorted trigonal bipyramidal geometry. Antibacterial activities of the compounds were evaluated using the disk diffusion method against six bacteria and Candida albicans. The Hg(II) complex shows superior activity toward S. epidermidis and E. coli whereas the other complexes are ineffective except the Co(NO3)2 complex: it showed weak activity toward all of the microorganisms. 相似文献
15.
[Co7(μ4‐O)2(O2C–CH3)8(NCO)2(HNPEt3)4] · 2 OEt2, a Seven Nuclearity Complex with Four, Five, and Sixfold Coordinated Cobalt Atoms The title compound was prepared from cobalt(II) acetate with Me3SiNPEt3 at 180 °C and subsequent crystallization from diethylether to give blue, moisture sensitive single crystals, which were characterized by a crystal structure determination. Space group P21/n, Z = 2, lattice dimensions at –80 °C: a = 1544.0(1), b = 1522.1(2), c = 1702.0(1) pm, β = 103.911(10)°, R = 0.0490. [Co7(μ4‐O)2(O2C–CH3)8(NCO)2 · (HNPEt3)4] has a centrosymmetric cluster‐like structure in which the octahedrally coordinated central cobalt atom is connected with the remaining six cobalt atoms via two μ4‐oxygen atoms as well as via four bridging acetato groups to form a Co(Co)6 octahedral skeleton. Four of the peripheric cobalt atoms have a distorted trigonal‐bipyramidal coordination sphere, the other two cobalt atoms are tetrahedrally coordinated. The latter are connected with the nitrogen atoms of the cyanato groups. 相似文献
16.
18‐crown‐6(18‐C‐6) complexes with K2[M(SeCN)4] (M = Pd, Pt): [K(18‐C‐6)]2[Pd(SeCN)4] (H2O) ( 1 ) and [K(18‐C‐6)]2[Pt(SeCN)4](H2O) ( 2 ) have been isolated and characterized by elemental analysis, IR spectroscopy and single crystal X‐ray analysis. The complexes crystallize in the monoclinic space group P21/n with cell dimensions: 1 : a = 1.1159(3) Å, b = 1.2397(3) Å, c = 1.6003(4) Å, β = 92.798(4)°, V = 2.2111(8) Å3, Z = 2, F(000) = 1140, R1 = 0.0418, wR2 = 0.0932 and 2 : a = 1.1167(3) Å, b = 1.2394(3) Å, c = 1.5968(4) Å, β = 92.945(4)°, V = 2.2071(9) Å3, Z = 2, F(000) = 1204, R1 = 0.0341, wR2 = 0.0745. Both complexes form one‐dimensionally linked chains of [K(18‐C‐6)]+ cations and [M(SeCN)4]2— (M = Pd, Pt) anions bridged by K‐O‐K interactions between adjacent [K(18‐C‐6)]+ units. 相似文献
17.
Metal‐ and Substituent‐Dependent Structural Diversity in Cobalt and Nickel Isophthalate Coordination Polymers with Bis(4‐pyridylformyl)piperazine Tethers
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Hydrothermal reactions of nickel or cobalt nitrate with the dipyridylamide ligand bis(4‐pyridylformyl)piperazine (4‐bpfp) and either 5‐methoxyisophthalate (H2omeip) or 5‐methylisophthalate (H2mip) afforded a series of coordination polymers that were structurally characterized by single‐crystal X‐ray diffraction. Different synthetic conditions afforded the 1D chain phase {[Ni(Homeip)2(H2omeip)(bpfp)] · 2H2O}n ( 1 ) or the mutually inclined interpenetrated (4, 4) grid system in {[Ni(omeip)(bpfp)(H2O)] · 2H2O}n ( 2 ). The analogous cobalt phase {[Co(omeip)(bpfp)] · 3H2O}n ( 3 ) lacks bound water molecules, which enforces a non‐interpenetrated (4, 4) grid structure based on {Co2(OCO)2} dinuclear clusters. Similar clusters are seen in {[Co(mip)(bpfp)(H2O)2] · 3.5H2O}n ( 4 ), which manifests a 1D ribbon structural motif. Its nickel congener {[Ni(Hmip)2(bpfp)(H2O)2] · 2H2mip}n ( 5 ) also shows a 1D chain motif. A variable temperature magnetic susceptibility study indicates antiferromagnetic coupling within the dimeric units in 3 and 4 concomitant with single ion effects. Additionally, thermal degradation properties of these new materials are described. 相似文献
18.
Wei Han Ling Li Zhan‐Quan Liu Shi‐Ping Yan Dai‐Zheng Liao Zong‐Hui Jiang Pan‐Wen Shen 《无机化学与普通化学杂志》2004,630(4):591-596
Three new complexes [CuL(N3)2] ( 1 ), [CuL(SCN)2] ( 2 ), and [NiL(SCN)2] ( 3 ) (L = 1, 4, 7‐triisopropyl‐1, 4, 7‐triazacyclononane, [—NR—C2H4—NR—C2H4—NR—C2H4—], R = i‐Pr) have been synthesized and structurally characterized. The three complexes all crystallize in the monoclinic space group P21/n, with the unit cell parameters a = 9.100(5), b = 19.492(11), c = 11.646(6)Å, β = 94.526(9)° for 1 , a = 10.148(3), b = 13.611(5), c = 15.777(6)Å, β = 95.412(6)° for 2 and a = 9.270(7), b = 16.629(14), c = 14.886(12)Å, β = 101.217(15)° for 3 . The central copper(II) and nickel(II) ions are coordinated to five nitrogen atoms, three of which from the L and two from N3— or SCN—, forming a slightly distorted square pyramidal geometry. Moreover, elemental analysis, IR, UV‐vis and ESR spectra of complexes 1 ‐ 3 were also determined. 相似文献
19.
The new copper coordination polymers 2[CuX(μ‐2‐chlor‐opyrazine‐N, N')] (X = Cl ( I ), Br ( II ), 1[CuI(2‐chloropyrazine‐N)] ( III ) and [Cu2I2(2‐chloropyrazine)] ( IV ) has been prepared by the reaction of the copper(I) halides with 2‐chloropyrazine at roomtemperature or under hydrothermal conditions. The crystal structures of the 1:1 compounds I and II consist of zig‐zag CuX single chains running parallel to the crystallographic a‐axis which are linked by the 2‐chloropyrazine spacer molecules to sheets parallel to (010). For the iodine compound III a one‐dimensional structure is found which consists of CuX double chains running parallel to the crystallographic a‐axis. The thermic properties of all compounds were investigated in different gas atmospheres using simultaneously differential thermal analysis and thermogravimetry (DTA‐TG) as well as temperature resolved X‐ray powder diffraction. On heating, the 1:1 compounds I and II decompose directly to the corresponding copper(I) Halides, whereas the thermal decomposition of III occcur via IV as an intermediate. 相似文献
20.
《Journal of Coordination Chemistry》2012,65(11):1337-1351
The reaction of MX2 (M = Co(II), Ni(II); X = Cl, Br) with 2-aminopyrimidine in aqueous acid yields compounds [(2-apmH)2MX4], (2-apmH)2[MX4], or (2-apmH2) [MX2(H2O)4]X2 (2-apmH = 2-aminopyrimidinium; 2-apmH2 = 2-aminopyrimidinium(2+)). All compounds have been characterized by single crystal X-ray diffraction. The compounds [(2-apmH)2MX4] with M = Co, X = Cl (1); M = Ni, X = Cl (3); and M = Ni, X = Br (4) are isomorphous and crystallize as nearly square planar MX4 units with the 2-apmH cations coordinated in the axial sites through the unprotonated ring nitrogen. (2-ApmH)2[CoBr4] (2) crystallizes as the salt with a nearly tetrahedral CuBr4 2- anion. (2-ApmH2)[NiBr2(H2O)4]Br2 (5) forms as a cocrystal of the neutral, six-coordinate nickel complex and (2-ampH2)Br2, stabilized by extensive hydrogen bonding. Crystal data (1): monoclinic, P21/c, a = 7.540(4), b = 12.954(4), c = 7.277(3) Å, β = 110.09(6), V = 667.4(5) Å3, Z = 2, Dcalc = 1.955 Mg/m3, μ = 2.079 mm-1, R = 0.0501 for [|I|≥2(I)]. For (2): triclinic, P-1, a = 7.720(2), b = 7.916(2), c = 14.797(3) Å, α = 97.264(3), β = 104.788(3), γ = 105.171(3)°, V = 825.3(3) Å3, Z = 2, Dcalc = 2.296 Mg/m3, μ = 10.715 mm-1, R = 0.0308 for [|I|≥2(I)]. For (3): monoclinic, P21/c, a = 7.595(3), b = 12.891(4), c = 7.204(3) Å, β = 111.07(3)°, V = 658.2 Å3, Z = 2, Dcalc = 1.982 Mg/m3, μ = 2.279 mm-1, R = 0.0552 for [|I|≥2(I)]. For (4): monoclinic, P21/c, a = 7.840(2), b = 13.358(4), c = 7.518(2) Å, β = 110.923(3)°, V = 938.6(3) Å3, Z = 2, Dcalc = 2.577 Mg/m3, μ = 12.18 mm-1, R = 0.0280 for [|I|≥2(I)]. For (5): orthorhombic, Pnma, a = 16.776(6), b = 11.943(4), c = 7.079(3) Å, V = 1418.2(9) Å3, Z = 4, Dcalc = 2.564 Mg/m3, μ = 12.639 mm-1, R = 0.0381 for [|I|≥2σ(I)]. 相似文献