Synthesis,characterization and crystal structure of a 3‐D supramolecular Cu/Mn complex with pydc

A supramolecular compound, {[CuMn(pydc)₂(H₂O)₅]·2H₂O} ( 1 ) (pydc = pyridine‐2,6‐dicarboxylate dianion), has been synthesized and characterized by single‐crystal X‐ray diffraction. Single‐crystal X‐ray analysis reveals that it crystallizes in the triclinic space group P‐1, a = 8.4763(17) Å, b = 9.7715(19) Å, c = 13.909(3) Å, α =101.234(3)°, β =102.520(3)°, γ= 97.375(4)°. Two mixed‐metal ions exhibit similar coordinated geometries with octahedron. 1 possesses a 3‐D unusual supramolecular network featuring 1D water tape. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and structure of a new one‐dimensional cobalt complex with dicyanamide and 4‐picolyl choride bridges

The synthesis and structure of the 1D cobalt (II) complex, [Co( L )₂(dca)₂] ( 1 ) (dca = dicyanamide, C₂N₃^–, L = 4‐picolyl choride) is reported. Complex 1 crystallized in triclinic system, space group P ‐1, with cell dimensions of a = 7.291(2) Å, b = 7.481(2) Å, c = 9.007(3) Å, α =104.444(4)°, β = 96.971(4)°, γ =102.618(4)°, V = 456.1(2) ų, Z = 1, Dc = 1.624 Mg/m³. In complex 1 , Co (II) is 6‐coordinated by N atoms of four dca ligands and two L ligands. The centrosymmetric CoN6 chromophore is an axially elongated octahedron that has Co‐N distances ranging from 2.122(3) to 2.154(3) Å. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structures of N1, N5‐dibenzoyltetrahydro‐4‐methyl‐1, 5‐benzodiazepin‐2‐one (DBTBO) and tetrahydro‐4‐methyl‐1, 5‐benzodiazepin‐2‐one (TBO)

Adducing structural analogies between the two fused systems, N1, N5‐Dibenzoyltetrahydro‐4‐methyl‐1,5‐benzodiazepin‐2‐one, C₂₄H₂₀N₂O₃ (DBTBO CCDC 200341) and Tetrahydro‐4‐methyl‐1,5‐benzodiazepin‐2‐one, C₁₀H₁₂ N₂O (TBO CCDC 200342) helps to find the pharmacological differences from the view point of variant hetero atom substitutions in the hetero cycle. Both the diazepines crystallized in identical monoclinic space group P2₁/n with a = 14.1134(1) Å, b = 9.2444(1) Å, c = 16.3812(1) Å; β = 107.11(1)º, V = 2042.7(3) ų for DBTBO and a = 9.3363(7) Å, b = 10.4895(8) Å, c = 9.9852(7) Å, β = 91.314(1)º, V = 977.62(1) ų for TBO, respectively. The two structures were solved by direct methods and refined by full‐matrix least‐squares procedure to final R‐values of R1 = 0.0575(DBTBO) and R1 = 0.0984(TBO). Structural differences include non‐identical boat conformations of these seven‐membered rings and the different non‐bonding interactions in the benzodiazepine pair.     

Crystal Structure of 5,6‐Dinitrobenzimidazole.monohydrate

The title compound (C₇H₆N₄O₅) crystallizes in the monoclinic space group P2₁/c with a=8.566(1) Å, b=14.493(3) Å, c=7.583(1) Å, β=87.75(1)°, V=940.7(3) ų, Z=4, D_x=1.597 g.cm^‐3. The structure was solved by direct methods and refined by full‐matrix least‐squares method (R=0.0696). The title compound consists of an imidazole ring with the two NO₂ groups and one water molecule. The short inter‐ molecular N‐H^…N [2.03(5) Å] and O_water‐H^…O [1.98(5) Å] hydrogen bonds are highly effective in holding the molecule in a stable state as a whole.     

Crystal structure of strontium aqua(ethylenediaminetetraacetato)cobaltate(II) tetrahydrate Sr[CoEdta(H2O)] · 4H2O

The complex Sr[Co^II Edta] · 5H₂O (I) (where Edta ^4? is the ethylenediaminetetraacetate ion) has been synthesized. The crystal structure of this compound is determined by X-ray diffraction. Crystals are monoclinic, a = 7.906(2) Å, b = 12.768(2) Å, c = 18.254(3) Å, β = 95.30(3)°, V = 1834.8 ų, space group P2₁/n, Z = 4, and R = 0.036. The structure is built up of the binuclear complex fragments {Sr(H₂O)₃[CoEdta(H₂O)]}, which consist of the anionic [CoEdta(H₂O)]^2? and cationic [Sr(H₂O)₃]²⁺ units linked by the Sr-O bonds into a three-dimensional framework. The coordination polyhedra of the Co and Sr atoms are mono-and bicapped trigonal prisms. The coordination sphere of the Co atom (the coordination number is equal to 6 + 1) involves six donor atoms (2N and 4O) of the Edta ^4? ligand and the O_w atom of water molecule. One of the Co-O distances (2.718 Å) is considerably longer than the other Co-O_lig distances (2.092–2.190 Å) and the Co-O_w(1) distance (2.079 Å). The Sr coordination polyhedron (the coordination number is eight) contains three water molecules, three carbonyl O atoms of the three different anionic complexes, and two O atoms of one acetate group of the fourth anionic complex. The Sr-O distances fall in the range 2.535–2.674 Å. The structural formula of the compound is {Sr(H₂O)₃[CoEdta(H₂O)]}_3∞ · H₂O.     

Synthesis,characterization and magnetic behaviour of a linear chain poly(oxomolybdophosphate) compound

A new linear chain compound, [Cu(en)₂][Cu(en)₂(H₂O)_1.5][Cu(en)₂(H₂O)₂]_0.5[{Cu(en)₂}₅{HP₂Mo₅O₂₃}₃] · 6.5H₂O ( 1 ) (en = ethylenediamine), has been synthesized under mild hydrothermal conditions, and characterized by elemental analysis, IR, thermogravimetric analyses, magnetic susceptibility measurements and single‐crystal X‐ray diffraction. The crystals are monoclinic, C2/c, a = 42.509(2) Å, b = 25.542(2) Å, c =22.1011(14) Å, β = 102.5940(10)º, V = 23419(3) ų, Z = 8. The crystal structure of 1 features Cu‐bearing cations that are both free as well as being coordinated to the poly(oxomolybdophosphate) groups formed a linear chain that runs along the b axis. Magnetic studies show that the complex is antiferromagnetic. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and structure of the three‐dimensional coordination polymer [Ag3hmt3(μ3 ‐btc)]·5H2O

A new coordination polymer, [Ag₃hmt₃(μ₃ ‐btc)]·5H₂O (1) (hmt = hexamethylenetetramine, btc=1,3,5‐benzenetricarboxlic), has been successfully synthesized. Crystal data: P2₁/a, a = 11.9906(2) Å, b = 17.3689(2) Å, c = 16.96100(10) Å, β = 101.9820(14)°, V = 3455.40(7) ų, Z = 4, Dc = 2.002 Mg/m³. In the hexagonal structure of Ag‐hmt unit, each Ag‐hmt unit comprises three Ag atoms and three hmt ligands. The μ₃ ‐btc ligands bridge adjacent two‐dimensional honeycomb‐like Ag‐hmt layers to form three‐dimensional networks. Structure analysis show that hydrogen bonds play a key role for the stable structure in the compounds. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Powder study of propanthioamide dervative C8H6N2S2

The crystal structure of 2‐cyano‐3‐(2‐thienyl)prop‐2‐enethioamide (C₈H₆N₂S₂), a propanethioamide derivative was solved from high resolution laboratory X‐ray powder diffraction data collected at ambient conditions. Structure determination was performed by means of the global optimization method of simulated annealing at a resolution of 1.5 Å. Rietveld refinement yielded an R_WP value of 4.02% (P2₁/a, a = 15.8174(2) Å, b = 5.6502(1) Å, c = 11.0952(1) Å, β = 116.9923(7)°, V = 883.6(5) ų, Z = 4). The molecules are stacked in parallel layers and are stabilized by hydrogen bonds. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,crystal structure and photophysical studies on a ruthenium(II) carbonyl hydrido compound based on 2,2′‐bipyridyl‐5,5′‐dicarboxylic acid (H2bpdc)

A novel complex, namely [Ru^II(PPh₃)(CO)(H)(Hbpdc)]·2MeOH ( 1 ) (H₂bpdc = 2,2′‐bipyridyl‐5,5′‐dicarboxylic acid), has been synthesized from the reaction of H₂bpdc with [Ru^II(PPh₃)₃(CO)(H)₂] in methanol under mild condition and characterized by elemental analysis, IR spectrum, ESI mass spectrometry, and single crystal X‐ray diffraction. The structure shows that the complex crystallizes in the monoclinic space group P2₁/c with unit cell parameters a = 11.8984(13) Å, b = 16.5180(18) Å, c = 25.5322(19) Å, β = 115.302(4)°, V = 4536.6(8) ų, Z = 4. This compound features a 1‐D supramolecular chain constructed via hydrogen bonds. Its photophysical properties have been investigated in MeOH solution and in the solid state at room temperature.     

Crystal structure of 2‐(2'‐hydroxyphenyl)‐6‐tributylstannyl‐4‐(3H )‐quinazolinone and 2‐(2'‐hydroxyphenyl)‐6‐iodo‐4‐(3H)‐quinazolinone

The structures of the title compounds C₂₆H₃₇N₂O₂Sn ( I ) and C₁₄H₉IN₂O₂ ( II ) were determined by single‐crystal X‐ray diffraction technique. Compound I crystallizes in the triclinic space group P1 with a = 9.560(3) Å, b = 16.899(6) Å, c = 17.872(5) Å, α = 65.957(7)°, β = 83.603(5)°, γ ( = 75.242(5)°, V = 2549.8(13) ų, Z = 4, and D =1.374 g/cm³. The compound consists of a quinazolinone ring with phenol and tributylstannyl moieties. Compound II crystallizes in the monoclinic space group P2₁/c with a = 7.6454(12) Å, b = 5.9270(9) Å, c = 27.975(4) Å; α = 90°, β = 95.081(3)°, γ = 90°, V = 1262.7(3) ų, Z = 4, and D = 1.915 g/cm³. The compound consists of a quinazolinone ring with phenol and iodine substituents. For both I and II , the short intramolecular O–H…N and two long intermolecular N–H…O hydrogen bonds are highly effective in holding the molecular system in a stable state. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure and electrochemical property of one‐dimensional complex: [K(cis‐syn‐cis‐ dicyclohexyl‐18‐crown‐6)]2[Cu(mnt)2]

One metalorganic complex [K(cis‐syn‐cis‐ dicyclohexyl‐18‐crown‐6)]₂[Cu(mnt)₂] (mnt = maleonitriledithiolate) has been obtained by the reaction of dicyclohexyl‐18‐crown‐6 with K₂mnt and CuCl₂·2H₂O. The title complex has been characterized by elementary analysis, FT‐IR, UV‐Vis spectroscopy and x‐ray single crystal diffraction. The title complex crystallizes in the triclinic space group P1 with crystallographic data: a = 10.870(6) Å, b = 11.536(6) Å, c = 12.904(7) Å, α = 101.541(10)°, β = 110.573(9)°, γ = 99.441(9)°, V = 1435.2(13) ų, Z = 1, D_calcd = 1.350 g/cm³, F(000) = 615, R₁ = 0.0641, wR₂ = 0.1475. It displays one‐dimensional chain‐like structure formed by [K(cis‐syn‐cis‐ dicyclohexyl‐18‐crown‐6)]⁺ complex cations and [Cu(mnt)₂]^2‐ complex anions through N‐K‐N interactions. Its electrochemical behavior has also been studied by the cyclic voltammetry. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structures of strontium and barium ethylenediaminetetraacetato cobaltates(III), Sr[CoEdta]2·9H2O and Ba[CoEdta]2·8H2O: Comparison of the structures of complexes in the series M’[CoEdta]2·nH2O (M’ = Mg, Ca, Sr, Ba; n = 7–10)

Cobalt(III) complexes, namely, Sr[CoEdta]₂·9H₂O (I) and Ba[CoEdta]₂·8H₂O (II) (where Edta ^4- is the ethylenediaminetetraacetate ion), are synthesized. The crystal structures of these compounds are determined using X-ray diffraction. Crystals of compound I are triclinic, a = 6.514(1) Å, b = 11.410(2) Å, c = 12.317(2) Å, α = 67.87(1)°, β = 88.73(2)°, γ = 84.22(2)°, V = 843.63(3) ų, Z = 1, space group P1, and R = 0.0295 for 4130 reflections with I > 2σ(I). Crystals of compound II are monoclinic, a = 6.543(2) Å, b = 12.895(3) Å, c = 19.489(4) Å, β = 95.24(3)°, V = 1637.5(5) ų, Z = 2, space group P2₁, and R = 0.050 for 3016 reflections with |F| > 3σ(|F|). The structures of compounds I and II are compared with those of the previously studied complexes Mg[CoEdta]₂·10H₂O (III) and Ca[CoEdta]₂·7H₂O (IV). The crystal structure of the cobalt(III) complex with the strontium cation (I) is topologically similar to the crystal structure of cobalt(III) complex with the calcium cation (IV). The former structure is built up of the two symmetrically independent homochiral anionic complexes [CoEdta]^? (A _I and B _I), the aqua cations [Sr(H₂O)₈]²⁺, and the molecules of crystalization water w _cr. The structure of compound II involves two independent anions [CoEdta]^? (A _II and B _II) with different chiralities (i.e., they are kryptoracemates). The A _II anions are linked via the barium cations into {Ba(H₂O)₇[CoEdta]} _1∞ ⁺ chain agglomerates due to the incorporation of two terminal oxygen atoms O_u of the anions neighboring in the chain into the coordination sphere of the barium atom. All four structures (I–IV) contain stacks composed of the [CoEdta]^? homochiral anions forming layers aligned parallel to the (001) plane. The aqua cations [Sr(H₂O)₈]²⁺, [Mg(H₂O)₆]²⁺, and [Ca(H₂O)₇]²⁺ or the partially hydrated barium cations [Ba(H₂O)₇(O_u)₂]²⁺ (in structure II), as well as water molecules w _cr, are located between the anion layers. The octahedral environment of the cobalt(III) atoms consists of donor atoms (2N and 4O) of the Edta ^4? ligand. The Co-N bonds in the A _I, B _I, A _II, and B _II anions [the mean bond lengths are 1.927(4), 1.921(4), 1.910(6), and 1.921(6) Å, respectively] are considerably longer than the Co-O bonds [the mean bond lengths are 1.908(5), 1.902(5), 1.904(6), and 1.908(6) Å, respectively]. The mean distances Sr-O_w and Ba-O_w in the strontium and barium polyhedra are 2.609(4) and 2.834(8) Å, respectively. The mean distance Ba-O_u is 2.814(7) Å.     

Three‐Dimensional Structure Constructed via Hydrogen Bonds and π‐π Stacking Interaction. Crystal Structure of [Cu(AFO)2(H2O)2](ClO4)2.2(AFO).2H2O (AFO = 4,5‐Diazafluoren‐9‐one)

The structure of the title complexes [Cu(AFO)₂(H₂O)₂](ClO₄)₂.2(AFO).2H₂O (AFO = 4,5‐Diazafluoren‐9‐one)has been established by single‐crystal X‐ray diffraction. The complex crystallizes in the triclinic space group P‐1 with cell constants a = 7.659(3) Å, b = 11.066(3) Å, c = 14.203(5) Å, alpha = 75.16(3)°, β = 79.87(3)°, gamma = 85.71(3)°, Z = 1. The structure was solved by direct methods and refined to R₁ = 0.0595 (wR₂ = 0.1164). The X‐ray analysis reveals that a pair of AFO ligands chelate to a Cu(II) atom in an asymmetric fashion with one Cu‐N bond being much longer than the other, the Cu(II) atom is further coordinated by a pair of aqua ligands to form an elongated octahedral geometry. In the crystal of the complex, the mononuclear complex cations [Cu(AFO)₂(H₂O)₂]²⁺, uncoordinated AFO molecules, lattice water molecules and perchlorate anions are assembled into 3‐D structure via hydrogen bonds and π‐π stacking interaction.     

Two organic‐inorganic hybrids with Keggin polyanions

Two new Keggin polyoxometalates [Co(phen)₃]₂[SiW₁₂O₄₀]·6H₂O (1) and (ppy)₆ H₄SiMo₁₂O₄₀·0.4H₂O (2) (phen = 1,10′‐phenanthroline, ppy = 4‐(5‐phenylpyridin‐2‐yl)pyridine) have been synthesized by the hydrothermal method. Single crystal X‐ray analysis revealed that compound 1 crystallizes in the monoclinic crystal system with cell parameters of a = 13.344(2) Å, b = 17.191(3) Å, c = 22.002(4) Å, α = 90.00°, β = 99.566(2)°, γ = 90.00°, V = 4977 ų, Z = 2, and compound 2 crystallizes in the triclinic crystal system with cell parameters of a = 11.297(2) Å, b = 12.341(3) Å, c = 19.354(4) Å, α = 107.60(3)°, β = 95.80(3)°, γ = 94.16(3)°, V = 2543.7(9) ų, Z = 1. Both 1 and 2 represent organic ligand molecules and inorganic Keggin anions, which are further interconnected to a 3D framework by supramolecular interactions. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of N‐(2‐methoxyphenyl)‐3,6‐diphenyl‐1,4‐dihydro‐1,2,4,5‐tetrazine‐1‐carbonamide

The title compound, C₂₂H₁₉N₅O₂, was prepared and its structure was determined by X‐ray diffraction [CCDC 216074]. The compound crystallizes from ethanol in the orthorhombic system, space group P2₁2₁2₁, with unit cell parameters: a =10.048(1) Å, b = 13.935 (2) Å, c =14.607(2) Å, Z =4, and V=2045.3(5) ų. The crystal structure was solved by direct methods and refined by full‐matrix least‐squares to a final R‐value of 0.0516 with 3621 unique reflections. The central six‐membered ring of the compound has a boat conformation and is not homoaromatic, in which adjacent atoms N1 and N4 deviate from the plane of the ring by 0.4546(33) Å and 0.3786(33) Å, respectively. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of 1‐allyl‐5‐(4‐methylbenzoyl)‐4‐(4‐methylphenyl)pyrimidine‐2(1H)‐thione

The crystal structure of 1‐allyl‐5‐(4‐methylbenzoyl)‐4‐(4‐methylphenyl)pyrimidine‐2(1H)‐thione (C₂₂H₂₀N₂OS) has been determined from three dimensional single crystal X‐ray diffraction data. The title compound crystallizes in the monoclinic space group P 2₁/c, with a = 10.6674(13), b = 10.1077(7), c = 17.9467(19) Å, β = 98.460(9)°, V = 1914.0(3) ų, D_calc = 1.251 g cm^–3, Z = 4. In the title compound, the allyl group shows positional disorder. Molecules are linked by C‐H···O, C‐H···N and C‐H···S intermolecular interactions forming two‐dimensional network. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structures of four inclusion compounds of 2,2′-dithiosalicylic acid and tetraalkylammonium

Herein four inclusion compounds of 2,2′-dithiosalicylic acid and tetraalkylammonium, 2(CH₃)₄N⁺·C₁₄H₈O₄S₂^2?·H₂O (1), (C₂H₅)₄N⁺·C₁₄H₉O₄S₂^?·0.25H₂O(2), (n-C₃H₇)₄N⁺·C₁₄H₉O₄S₂^? (3) and (n-C₄H₉)₄N⁺·C₁₄H₉O₄S₂^?(4) are prepared and characterized by X-ray single crystal diffraction. As shown in the results, compounds 1 and 3 belong to orthorhombic crystal system with different space groups of P2₁2₁2₁ and Pca2₁, and 2 and 4 are monoclinic system with similar groups of P2₁/n and P2₁/c. The crystallography data are displayed below: 1: a = 10.5903(7) Å, b = 10.6651(7) Å, c = 21.9476(13) Å, V = 2478.9(3) ų, Z = 4, R₁ = 0.0359; 2: a = 8.13340(1) Å, b = 22.0741(3)Å, c = 13.2143(2)Å, β = 101.6360(1) °, V = 2323.70(6) ų, Z = 1, R₁ = 0.0385; 3: a = 15.7857(2) Å, b = 8.24830(1) Å, c = 20.2599(2) Å, V = 2637.94(5) ų, Z = 4, R₁ = 0.0308_degree4: a = 11.7476(2) Å, b = 17.1346(1) Å, c = 16.3583(3)Å, β = 109.4560(1) °, V = 3104.74(9)ų, Z = 4, R₁ = 0.0562. Interestingly, although the carbon chains of the guest templates vary from methyl group to butyl group, the host molecules of 2,2′-dithiosalicylic acid all construct the similar 2D hydrogen-bonded host layers with or without the existence of water molecules to contain the guest templates to yield analogous sandwich-like inclusion compounds. Obviously, although the guest templates will have certain effects on the ultimate formation of these crystal structures, the host molecule of 2,2′-dithiosalicylic acid is a controlling factor to form these four inclusion compounds.     

Solvothermal syntheses and crystal structures of two 4‐heterocyclic acylpyrazolone complexes

Many explorations of transition metal (M)‐L system under solvothermal condition, have led to the syntheses of two new 4‐heterocyclic acylpyrazolone complexes [Co(L)₂(CH₃OH)₂] (HL = 1‐phenyl‐3‐methyl‐4‐(2‐furoyl)‐5‐pyrazolone) ( 1 ) and [Cr(L)₃] ( 2 ). Single‐crystal X‐ray analyses reveal that crystal structures of compound 1 and 2 are respectively orthorhombic, Pbca, a = 15.0378(6) Å, b = 9.8405(4) Å, c = 20.7321(8) Å, V = 3067.9(2) ų, Z = 8 and triclinic, P‐1, a = 10.7966(18) Å, b = 13.023(2) Å, c = 15.520(3) Å, α = 73.011(4)°, β = 84.884(4)°, γ = 70.267(4)°, V = 1964.3(6) ų, Z = 2. Complex 1 has a two‐dimensional (2D) network structure that is formed by O–H···N H‐bonding interactions. Complex 2 makes a one‐dimensional (1D) zigzag chain structure by intermolecular π···π interactions, which is further interlinked via C–H···N H‐bonding interactions to generate a 2D sheet, and then a three‐dimensional (3D) supramolecular network structure is further linked by intermolecular C–H···π interactions. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure analysis of N,N′‐bis(salicylidene)‐2‐methyl‐1,2‐propanediaminato‐nickel(II)

In the title compound, N,N′‐Bis(salicylidene)‐2‐methyl‐1,2‐propanediaminato‐nickel(II), [NiC₁₈H₁₈N₂O₂], (CCDC 235278), the Ni^II atom is coordinated by two iminic N and two phenolic O atoms of the N,N′‐Bis(salicylidene)‐2‐methyl‐1,2‐propanediaminate (SALPD^2‐) ligand. The geometry of the coordination sphere around the Ni atom is distorted square‐planar. Ni(II) ion, forms crystals which belong to the orthorhombic system, space group P cab, with unit cell dimensions a=11.5531(1), b=15.985(4), c=17.418(1) Å, V=3210.5(9) ų. The cell contains eight molecules. The contact distance Ni...Ni^a between the neighbouring molecules is 4.4704(8) Å. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Synthesis,characterization and crystal structure of a novel 3‐D copper(II) polymer with bent N‐containing ligand

An exploration of the mixed‐ligand system under hydrothermal condition, has led to the isolation of a 3‐D novel framework {[Cu₂(mp)L₂)(H₂O)₂]·6H₂O}_n ( 1 ) (mp = benzene‐1,2,4,5‐ tetracarboxylate tetraanion, L = 4‐(5‐(pyridin‐4‐yl)‐1,3,4‐thiadiazol‐2yl)pyridine). Single‐crystal X‐ray analyses reveal that it crystallizes in the triclinic space group P‐1, a = 8.807(4) Å, b =11.139(6) Å, c = 11.291(5) Å, α=75.337(7), β = 73.584(5), γ= 66.795(5)°. The Cu^II ions are linked into an extended 2‐D grid net via mp molecules. Further these layers are united together through the bridging L to form a 3‐D structure, which exhibits a new 4‐connected topological network. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)