Synthesis and crystal structure of 4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane bis[dichloro(thiocyanato)copper(II)]

A new complex salt [4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane bis[dichloro(thiocyanato)copper(II)], [H₂(Crypt-222)][CuCl₂(SCN)]₂, is synthesized and studied by X-ray diffraction analysis. The crystals are monoclinic (space group C2/c, a = 14.603 Å, b = 8.330 Å, c = 25.091 Å, β = 100.76°, Z = 4). The structure is solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.047 for 2943 independent reflections (CAD-4 automated diffractometer, λMoK _α radiation). The Cu²⁺ cations and Cl^? and SCN^? anions form infinite polymeric chains of spiro-conjugated alternating centrosymmetric four-membered CuCl₂Cu cycles and eight-membered Cu(SCN)₂Cu cycles through coordination bonds. The coordination polyhedron of the Cu²⁺ cation is a distorted trigonal bipyramid. The [H₂(Crypt-222)]²⁺ dication contains trifurcate N⁺-(…O)₃ bonds on axis 2.     

Hirshfeld Surface Analysis,Crystal Structure and Spectroscopic Studies of a New Cu(II) Halocuprate Salt with Protonated N-Amino-Ethyl-Piperazine

(C₆H₁₈N₃)₄[CuCl₅]₂[CuCl₄]₃·1.42H₂O is prepared and characterized by various physicochemical techniques. The single crystal X-ray diffraction structural analysis reveals that the title compound belongs to the orthorhombic system with the space group Cmca. Its unit cell dimensions are: a = 24.286(2) Å, b = 14.3082(14) Å, c = 16.6160(16) Å, Z = 4, V = 5773.8(10) ų. Its crystal structure is determined and refined down to R = 0.024 and wR(F²) = 0.059. The structure contains three crystallographically independent Cu²⁺ ions coordinated to chlorine anions in various fashions. Cu1 is five-coordinated in a distorted square pyramidal fashion, while Cu2 and Cu3 are four-coordinated in square planar and distorted tetrahedral fashions, respectively. The entities are interconnected by means of the hydrogen bonding [O(W)–H…Cl, N–H…Cl, C–H…Cl and C–H…O(W)], forming a three-dimensional network. Intermolecular interactions are investigated by Hirshfeld surfaces and the contacts of the eight different chloride atoms are notably compared. The vibrational absorption bands are identified by infrared spectroscopy. The optical study is performed by UV-vis absorption.     

Synthesis and structure of bis(1,2-diaminoethane) copper(II) bis(<Emphasis Type="Italic">o</Emphasis>-hydroxybenzoate) monohydrate and <Emphasis Type="Italic">trans</Emphasis>-diaquabis(1,2-diaminoethane)copper(II) bis(<Emphasis Type="Italic">o</Emphasis>-aminobenzoate)

X-ray structural analysis has been performed for two complex compounds: Cu(en)₂(o-HB)₂H₂O (I) (a = 16.873(4) Å, b = 8.713(2) Å, c = 14.803(3) Å, β = 91.15(2)°, V = 2175.8(8) ų, C2/c, Z = 4, R(F) = 0.0263, 1516 reflections with I > 3σ (I)) and [Cu(en)₂(OH₂)₂]²⁺(o-AB^?)₂ (II) (a = 7.488(5) Å, b = 22.122(8) Å, c = 7.856(5) Å, β = 118.77(2)°, V = 1140.7(11) ų, P2₁/n, Z = 2, R(F) = 0.0432, 1684 reflections with I > 3σ(I)) synthesized under identical conditions (en is ethylenediamine, o-HB is o-hydroxybenzoate, and o-AB is o-aminobenzoate). Although the compounds were assumed to have similar structures and the Cu-Lig bond lengths and the cis and trans angles are acceptable for an octahedral structure, the geometric parameters of o-HB suggest that the copper atom has a plane square environment.     

Reaction of copper(II) cysteinate with thiosemicarbazide: Crystal structure of a complex of copper(II) thiocyanate with thiosemicarbazide

The reaction of copper(II) cysteinate with thiosemicarbazide (TSC) in water was found to yield complex of copper(II) thiocyanate of the [Cu(TSC)₂(SCN)₂] composition, whose crystal structure was determined by X-ray crystallography. Crystals of the complex are triclinic with a = 6.040 Å, b = 7.112 Å, c = 8.276 Å, α = 91.34°, β = 101.72°, Γ = 114.83°, Z = 2, space group \(P\bar 1\). Structural units of the complex are [Cu(TSC)₂]²⁺ centrosymmetric cations and (SCN)^? anions linked by hydrogen bonds (HB), as well as by electrostatic and π-π stacking interactions. The coordination polyhedron of Cu atoms is a square completed to bipyramid; the bonds Cu(1)-N(3), Cu(1)-S(1), and Cu(1)-S(2) are 2.002 Å, 2.303 Å, and 3.015 Å, respectively.     

Crystal and molecular structure of (hexafluoroacetylacetonato) (pivaloylacetonato)copper(II)

The crystal structure of (hexafluoroacetylacetonato)(pivaloylacetonato)copper(II) has been determined. Crystal data for CuO₄C₁₃H₁₄F₆: a = 8.288(2) Å, b = 8.682(2) Å, c = 12.307(2) Å; α = 90.75(3)°, β = 94.29(3)°, γ = 106.60(3)°; V = 845.7(3) ų, space group \(P\overline 1 \), Z = 2, d_calc = 1.617 g/cm³. The coordination polyhedron of the copper atom is formed by four oxygen atoms of two different β-diketonate ligands with Cu-O distances within 1.874–1.946 Å; the O-Cu-O bond angles are 94.8° and 90.6°. The complexes are united into centrosymmetrical “dimers” with Cu...Cu distances of 4.365 Å.     

Structure of A Coordination Polymer [Cu(En)<Subscript>2</Subscript>CrO<Subscript>4</Subscript>]<Subscript><Emphasis Type="Italic">n</Emphasis></Subscript>

The crystal structure of [Cu(En)₂CrO₄]_n (En is ethylenediamine) is determined: a = 14.7359(4) Å, b = 9.8083(3) Å, c = 14.2664(4) Å, V = 2061.98(10) ų, space group Cmce, Z = 8, d_x = 1.931 g/cm³. It is demonstrated that the studied phase is isostructural with [Сu(Еn)₂SO₄]_n. A pseudotetragonal copper atom coordination (Cu–N 2.0204 Å and 2.0244 Å, ∠N–Cu–N 84.73°) is completed to distorted octahedral by two oxygen atoms of chromate anions (Cu–O 2.433 Å and 2.380 Å).     

Triaqua(18-crown-6)strontium tetrachlorocuprate(II) hemihydrate: Synthesis and crystal structure

The new complex [Sr(18-crown-6)(H₂O)₃]²⁺[CuCl₄]^2? · 0.42H₂O was obtained; its crystal structure was determined by X-ray diffraction analysis: space group P2₁, a = 10.305 Å, b = 13.570 Å, c = 17.566 Å, β = 98.23 °, Z = 4 (direct method, anisotropic full-matrix least-squares method, R = 0.053 from independent reflections; CAD-4 automated diffractometer, λMoK _α). The asymmetric part of the unit cell comprises two independent “guest-host” complex cations [Sr(18-crown-6)(H₂O)₃]²⁺, two independent complex anions [CuCl₄]^2?, and a hydrate water molecule with a position population of 0.84(1).     

π-Complexes of Cu(I) with Alkynes. Synthesis and Crystal Structure of Cs[CuCl<Subscript>2</Subscript>(HOCH<Subscript>2</Subscript>C≡CCH<Subscript>2</Subscript>OH)] ⋅ H<Subscript>2</Subscript>O

Crystals of anionic π-complex Cs[CuCl₂(HOCH₂C≡CCH₂OH)] ? H₂O were synthesized by reaction of 2-butyne-1,4-diol with CuCl in a saturated aqueous solution of CsCl at 90°C and studied by X-ray diffraction analysis. The crystals are triclinic (space group \(P\bar 1\) ; a = 10.155(4) Å, b = 7.828(4) Å, c = 7.115(3) Å, α = 102.62(4)°, β = 100.77(3)°, γ = 106.71(4)°, V = 509(1) ų, Z = 2) and consist of stacks of individual anions [CuCl₂(HOCH₂C≡CCH₂OH)]^? and hydrated [Cs ? H₂O]⁺ cations between the stacks. The Cu(I) atom has trigonal surrounding of two Cl atoms and the C≡C bond of 2-butyne-1,4-diol molecule. The Cu-(C≡C) distance in the π-core is 1.905(8) Å; the C≡C bond is elongated to 1.223(11) Å. In addition to hydrogen bonds O-H?Cl, crystals of the complex also contain O(w)?H-O and O(w)?Cl bonds stabilizing their structure.     

Crystal structure and thermodynamic stability of an acetone solvate of bis(trifluoroacetylacetonato)copper(II)

A solvate [Cu(CF₃COCHCOCH₃)₂(CH₃COCH₃)] has been synthesized and characterized for the first time. According to X-ray structural data (diffractometer X8 APEX BRUKER, radiation MoK _α, T = 150 K), it crystallizes in the monoclinic crystal system, space group P2₁/c, a = 8.9940(4) Å, b = 22.3966(11) Å, c = 8.1884(3) Å, β = 92.705(2)°, V = 1647.59(12) ų, Z = 4, d _calc = 1.725 g/cm³, final R = 0.0272. The structure is molecular. In the equatorial plane the atom Cu(II) is surrounded with four oxygen atoms of two chelating ligands (CF₃COCHCOCH₃)^?; Cu-O distances 1.927–1.937 Å, O-Cu-O angles 86.18–93.30° and 170.18–175.67°. Square coordination of Cu is complemented to the square-pyramidal one by the oxygen atom of an acetone molecule behaving as an axial ligand; Cu-O_acetone 2.342 Å, O-Cu-O_acetone 89.66–100.11°. In the studied compound disorder of one of the chelate ligands implies the co-existance of the molecules in the cis- and trans-configuration in the crystal under ratio 54.6:45.4. In air the solvate rapidly degrades losing acetone, while in a sealed vessel melts around 313 K. Temperature dependence of equilibrium vapor pressure of acetone over the complex was measured with the static spoon gauge technique, thermodynamic characteristics of its dissociation process being derived: [Cu(CF₃COCHCOCH₃)₂(CH₃COCH₃)]_s = [Cu(CF₃COCHCOCH₃)₂]_s + CH₃COCH_3g, ΔH _av ⁰ = 49.6(3) kJ/mol, ΔS _av ⁰ = 152(1) J/(mol K), ΔG _av ⁰ = 4.30(2) kJ/mol.     

Synthesis and crystal structure of nickel(II) dinitrate molecular complex with 3,5-lutidine

Complex [Ni(NO₃)₂(3,5-lutidine)₃] (3,5-lutidine, 3,5-Lut-C₇H₉N) was synthesized, and its crystal structure was determined. Complex crystals are monoclinic: space group Cc, a = 14.445(1) Å, b = 10.024(1) Å, c = 17.607(1) Å, β = 108.96(1)°, V = 2411(1) ų, ρ_calcd = 2.389 g/cm³, Z = 4. The structure is built of discrete neutral complexes [Ni(3,5-Lut)₃(NO₃)₂]. The coordination sphere of Ni²⁺ ions is a disordered octahedron, which consists of three crystallographically nonequivalent lutidine ligands (Ni-N, 2.059–2.124 Å) and two oxygen ions of the two nitrate ions (Ni-O, 2.047–2.258 Å).     

Synthesis and crystal structure of a Cu(II) complex Cu<Subscript>2</Subscript>(Endc)<Subscript>2</Subscript>(Bipy)<Subscript>2</Subscript> and its photoluminescence properties

A novel Cu(II) complex Cu₂(Endc)₂(Bipy)₂ has been synthesized by the reaction of Cu(NO₃)₂ · 3H₂O, Endc (endo-norbornene-cis-5,6-dicarboxylic acid), and Bipy (2,2-bipyridine) at room temperature. Elemental analysis, IR spectra, and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. Crystal data for this complex: triclinic, P \(\bar 1\) with a = 9.0373(10), b = 10.1637(11), c = 10.5574(12) Å, α = 65.78(1)°, β = 72.32(2)°, β = 73.23(2)°, Z = 1, V = 827.46(16) ų, ρ _c = 2.160 g/cm³, F(000) = 410.0, R = 0.0483 and wR = 0.0958 independent reflections for 4468 observed ones (I > 2 σ(I)).The Cu²⁺ ion is coordinated by two nitrogen atoms from the Bipy molecule and three oxygen atoms from two Endc, giving a distorted squarepyramidal coordination geometry. Two neighboring Cu²⁺ ions are bridged by a pair of bimonodentate carboxyl groups of different Endc acids, giving a centrosymmetrical binuclear structure which a Cu…Cu distance of 3.2946 Å. The photoluminescence properties of the complex were studied at room temperature. The complex displays an obvious photoluminescent emission upon excitation at 390 nm in the solid state.     

Crystal structures of [Zn(SALIMP)(CH<Subscript>3</Subscript>CO<Subscript>2</Subscript>)]<Subscript>2</Subscript> and [Cu(SALIMP)Cl] with 2-[[(2-pyridinylmethyl) imino]methyl]phenol (HSALIMP) as a ligand

Two complexes [Zn(SALIMP)(CH₃CO₂)]₂ (1) and [Cu(SALIMP)Cl] (2) are obtained by the reactions of zinc(II) and copper(II) salts with a tridentate Schiff base ligand 2-[[(2-pyridinylmethyl) imino]methyl]phenol (HSALIMP). Their structure is determined by single crystal X-ray diffraction. Data for complex 1: C₃₀H₂₈N₄O₆Zn₂, CCDC number: 668213, M _r = 671.3, monoclinic, C2/c, with a = 34.670(5) Å, b = 15.266(2) Å, c = 23.464(4) Å, β = 114.045(2)°, V = 11341(3) ų, Z = 16, F(000) = 5504, GOOF(F ²) = 0.894, the final R = 0.0520 and wR = 0.1272 for 10515 observed reflections with I > 2σ(I); complex 2: C₁₃H₁₂N₂OClCu, CCDC number: 668211, M _r = 311.24, triclinic, P-1, with a = 7.4050(8) Å, b = 10.2369(11) Å, c = 16.2873(17) Å, α = 87.728(2)°, β = 87.818(2)°, γ = 78.279(2)°, V = 1207.4(2) ų, Z = 4, F(000) = 632, GOOF(F ²) = 1.077, the final R = 0.0326 and wR = 0.0381 for 4209 observed reflections with I > 2σ(I).     

Copper(I) π-complexes with 2-butyne-1,4-diol. Synthesis and crystal structure of (2-AmpH)[CuCl<Subscript>2</Subscript>(HOCH<Subscript>2</Subscript>C≡CCH<Subscript>2</Subscript>OH)] (2-AmpH<Superscript>+</Superscript> is 2-aminopyridinium cation)

Crystals of the π-complex (2-AmpH)[CuCl₂(HOCH₂C≡CCH₂OH)] (2-AmpH⁺ is the 2-aminopyridinium cation) were obtained by the reaction of 2-butyne-1,4-diol with CuCl in aqueous 2-aminopyridinium chloride solution and studied by X-ray diffraction: space group P \(\overline 1 \), a= 7.172(4), b= 7.796(3), c = 11.60(9) Å, α = 99.75(6)°, β = 96.53(7)°, γ = 101.03(3)°, Z = 2. The crystals consist of individual anions [CuCl₂(HOCH₂C≡CCH₂OH)]^? and cations [2-AmpH]⁺. The π-coordinated Cu(I) atoms of the complex anion have trigonal-planar surrounding of two chlorine atoms and C≡C bond of the 2-butyne-1,4-diol molecule. The alcohol groups form stable hydrogen bonds N-H?O (1.89 Å) and O-H?Cl (2.20 Å).     

Crystal structure and properties of polymeric hexaaqua-<Emphasis Type="Italic">hexakis</Emphasis>-(2-thiobarbiturato)-disamarium(III)

The structure (CIF file CCDC No. 1401886) of the hexaaqua-hexakis(2-thiobarbiturato)-disamarium [Sm₂(H₂O)₆(HTBA)₆] _n polymeric complex (I), where H₂ТВА is 2-thiobarbituric acid, is determined; its thermal decomposition and IR spectrum are studied. The crystals of I are monoclinic: a = 14.072(1) Å, b = 10.0842(6) Å, c = 15.323(1) Å, β = 110.408(2)°, V = 2037.9(2) ų, space group P2/n, Z = 2. All three independent thiobarbiturate anions HTBA^– coordinate to Sm³⁺ through oxygen atoms. To one of independent Sm³⁺ ions six (two terminal and four bridging) HTBA^– ions and two water molecules are coordinated; the second is bonded with four bridging HTBA^– and four water molecules, forming square antiprisms. The bridging HТВА–anions arrange antiprisms in layers. The structure is stabilized by hydrogen bonds and a π–π interaction between the HТВА^– ions. The topology of the polymer network of I is analyzed.     

Hexa(isothiocyanato)chromates(III) of Some Yttrium Group Lanthanide(III) and Europium Complexes with Nicotinic Acid: Synthesis and Crystal Structures

Double ionic complexes [M(C₅H₅NCOO)₃(H₂O)₂][Cr(NCS)₆] · nH₂O, where M = Eu (I), n = 1.15; Dy (II), Er (III), n = 1.5; M = Yb (IV), n = 2, have been synthesized by the reaction between M(NO₃)₃, M = Eu, Dy, Er, Yb, K₃[Cr(NCS)₆], and nicotinic acid (C₅H₅NCOO) in an aqueous solution and studied by chemical analysis, IR spectroscopy, and X-ray diffraction. Crystals of complexes I–IV are monoclinic, space group P2₁/n, Z = 4; a = 9.5358(2) Å, b = 25.4871(5) Å, c = 15.4303(4) Å, β = 105.513(1)°, V = 3613.6(1) ų, ρ_calcd = 1.799 g/cm³ for I, a = 9.5901(5) Å, b = 25.8599(15) Å, c = 15.6316(9) Å, β = 106.829(2)°, V = 3710.6(4) ų, ρ_calcd = 1.782 g/cm³ for II, a = 9.5640(3) Å, b = 25.8936(11) Å, c = 15.6498(7) Å, β = 106.895(2)°, V = 3708.3(3) ų, ρ_calcd = 1.791 g/cm³ for III, and a = 9.5049(2) Å, b = 25.6378(4) Å, c = 15.5120(3) Å, β = 106.934(1)°, V = 3616.1(1) ų, ρ_calcd = 1.864 g/cm³ for IV.     

Crystal structure of bis(semicarbazido)copper(II) nitrate [Cu(NH<Subscript>2</Subscript>NHC(O)NH<Subscript>2</Subscript>)<Subscript>2</Subscript>](NO<Subscript>3</Subscript>)<Subscript>2</Subscript>

The crystal structure of bis(semicarbazido)copper(II) nitrate [Cu(NH₂NHC(O)NH₂)₂](NO₃)₂ has been studied by X-ray diffraction. Monoclinic crystals, a = 6.835(2) Å, b = 7.733(2) Å, c = 10.320(3) Å, β = 105.701(3)°, V = 525.1(2) ų, space group P2₁/c, Z = 2, d _msd = 2.136 g/cm³, μ(MoK _α) = 2.143 mm⁻¹. The structure was solved with the program for automatic analysis of Patterson’s function and refined by full-matrix least squares in an anisotropic approximation for all non-hydrogen atoms using 753 independent reflections; R ₁ = 0.0203. The square environment of the Cu atom is formed from the amino nitrogen atoms of the hydrazine fragments and the C=O oxygen atoms of the two semicarbazide bidentate molecules (Cu-N 1.928 Å, Cu-O 1.999 Å). The axial positions are occupied by the O atoms of the NO ₃ ⁻ outer-spheric anions (Cu-O 2.505 Å). In the structure, the complex cations and the NO ₃ ⁻ anions are linked into a framework by N-H...O type hydrogen bonds. Original Russian Text Copyright ? 2007 by G. V. Romanenko, Z. A. Savelieva, and S. V. Larionov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No. 2, pp. 370–373, March–April, 2007.     

Spacer-armed binuclear copper(ii) complexes with salicylidene hydrazones of N-benzoylaminodicarboxylic acids

The structure and EPR spectra of copper(II) complexes with bis(salicylidene)hydrozones of N-benzoyl-L-aspartic and N-benzoyl-L-glutamic acids have been described. The compounds have been studied by chemical and thermal analyses, IR spectroscopy, and EPR spectroscopy. The molecular and crystal structure of the copper(II) complex with bis(salicylidene)hydrozone of N-benzoyl-L-aspartic acid (H₄L) of composition [Cu₂L · 2Py] · 2CH₃OH · H₂O has been determined by X-ray single-crystal diffraction. The crystals are monoclinic: a = 10.3316(7) Å, b = 16.7552(9) Å,c = 11.0137(6) Å, β = 105.758(3)°, space group P2₁, Z = 2. The complex has a polymeric structure composed of alternating copper-containing binuclear fragments bound to each other either via phenoxy bridges or via an aliphatic spacer (the Cu…Cu distances are 3.471 Å and 8.939 Å, respectively). The EPR spectra of the solutions of the complexes under study shows an isotropic signal comprising seven HFS lines due to two equivalent copper nuclei with the spin Hamiltonian parameters g = 2.115–2.122 and a _Cu = (36.1–36.9) × 10^?4 cm^?1, which indicates the reaization of weak exchange coupling of the paramagnetic centers.     

Structural characterization of a mixed-ligand complex of copper(II) with 1,10-phenanthroline and the <Emphasis Type="Italic">m</Emphasis>-aminobenzoate ion

A new copper(II) complex of 1,10-phenanthroline (C1₂H₈N₂) and the meta-aminobenzoate ion (m-amb; C₇H₆NO ₂ ^? ), having the formula Cu(C₁₂H₈N₂)(C₇H₆NO₂)Cl?0.5H₂O, is prepared and characterized by elemental analysis, IR spectroscopy, and single crystal X-ray diffraction. The structure is built up from monomeric units in which the coordination environment around the metal ion is a square plane arising from a bidentate 1,10-phenanthroline molecule, a monodentate m-amb anion, and a chloride ion. A very long (Cu–N = 2.856(5) Å) bond to the nitrogen atom of an adjacent m-amb ion generates [101] polymeric chains in the crystal. The crystal structure is consolidated by N–H???O and O–H???O hydrogen bonds and C–H???O, C–H???Cl, and aromatic π–π stacking interactions. Crystal data: C₁₉H₁₅ClCuN₃O_2.5, M _r = 424.33, monoclinic, P2₁/n (No. 14), a = 9.8200(5) Å, b = 10.9291(7) Å, c = 16.3803(9) Å, β = 105.293(3)°, V = 1695.74(17) ų, Z = 4, R(F) = 0.043, wR(F ²) = 0.122.     

Crystal structure and spectroscopic characterization of a coordination polymer of Copper(II) chloride with ethylenediamine and the 2-hydroxybenzoate ion

A new mixed-ligand one-dimensional copper(II) coordination polymer [Cu(en)(sal)Cl] _n where en = ethylenediamine(C₂H₈N₂) and Hsal = 2-hydroxybenzoic acid (salicylic acid; C₇H₆O₃) is synthesized and characterized by FTIR spectroscopy and single crystal X-ray diffraction. The structure contains Cu²⁺ ions in two different distorted octahedral coordination environments: an axially extended CuN₄Cl₂ moiety arising from a pair of bidentate en ligands and a CuO₄Cl₂ moiety arising from a pair of asymmetrically coordinated sal^– anions. The chloride ions bridge the copper ions into a zigzag chain propagating in [001]. The structure is consolidated by N–H???O and N–H???Cl hydrogen bonds which generate a layered network. Crystal data: C₉H₁₃ClCuN₂O₃, M _r = 296.20, monoclinic, P2₁/c, a = 13.9179(10) Å, b = 10.4900(8) Å, c = 8.5181(6) Å, β = 105.518(4)°, V = 1198.30(15) ų, Z = 4, R(F) = 0.026, w R(F ²) = 0.068.     

Crystal structures of copper(II) and zinc(II) complexes derived from 3-(2-pyridyl)pyrazole

Two dinuclear complexes [Zn(μ-L)(NO₃)(H₂O)]₂ (1) and [Cu₂(μ-L)₂(HL)₂](NO₃)₂(C₁₂H₈Br₂)_0.5·H₂O (2), (HL = 3-(2-pyridyl)pyrazole, C₁₂H₈Br₂ = 4,4′-dibromobiphenyl) are synthesized under hydrothermal conditions and characterized by elemental analysis and X-ray single crystal diffraction. Crystal data for 1: triclinic, \(P\bar 1\), a = 8.8478(7) Å, b = 15.0550(11) Å, c = 16.4310(12) Å, α = 107.588(4)°, β = 112.498(3)°, γ = 115.595(3)°, V = 2099.8(9) ų, Z = 2; for 2: triclinic, \(P\bar 1\), a = 7.2870(15) Å, b = 8.6840(17) Å, c = 9.3290(19) Å, α = 107.588(4)°, β = 112.498(3)°, γ = 115.595(3)°, V = 528.77(18) ų, Z = 1. Complex 1 and 2 are both dinuclear structures which are further packed into a 1D supramolecular chain and a 3D supramolecular framework via weak C–H…O hydrogen bond interactions respectively.