Sub-picogram determination of Vitamin B12 in pharmaceuticals and human serum using flow injection with chemiluminescence detection

A sensitive chemiluminescence (CL) method, based on the enhancive effect of cobalt(II) on the CL reaction between luminol and dissolved oxygen in a flow injection (FI) system, was proposed for determination of Vitamin B₁₂. The increment of the CL intensity was proportional to the concentration of Vitamin B₁₂, giving a calibration graph linear over the concentration from 2.0×10⁻¹⁰ to 1.2×10⁻⁶ g l⁻¹ (r²=0.9992) with the detection limit of 5.0×10⁻¹¹ g l⁻¹ (3σ). At a flow rate of 2.0 ml min⁻¹, a complete determination of Vitamin B₁₂, including sampling and washing, could be accomplished in 0.5 min with the relative standard deviations (R.S.D.) of less than 5.0%. The proposed method was applied successfully to the determination of Vitamin B₁₂ in pharmaceuticals, human serum, egg yolk and fish tissue.     

La3Ru8B6 and Y3Os8B6, new members of a homologous series R(A)nM3n−1B2n

Two new compounds, La₃Ru₈B₆ and Y₃Os₈B₆, were synthesized by arc melting the elements. Their structural characterization was carried out at room temperature on as-cast samples by using X-ray diffractometry. According to X-ray single-crystal diffraction results these borides crystallize in Fmmm space group (no. 69), Z=4, a=5.5607(1) Å, b=9.8035(3) Å, c=17.5524(4) Å, ρ=8.956 Mg/m³, μ=25.23 mm⁻¹ for La₃Ru₈B₆ and a=5.4792(2) Å, b=9.5139(4) Å, c=17.6972(8) Å, ρ=13.343 Mg/m³, μ=128.23 mm⁻¹ for Y₃Os₈B₆. The crystal structure of La₃Ru₈B₆ was confirmed from Rietveld refinement of X-ray powder diffraction data. Both La₃Ru₈B₆ and Y₃Os₈B₆ compounds are isotypic with the Ca₃Rh₈B₆ compound and their structures are built up from CeCo₃B₂-type and CeAl₂Ga₂-type structural fragments taken in ratio 2:1. They are the members of structural series R(A)_nM_3n−1B_2n with n=3 (R is the rare earth metal, A the alkaline earth metal, and M the transition metal). Structural and atomic parameters were also obtained for La_0.94Ru₃B₂ compound from Rietveld refinement (CeCo₃B₂-type structure, P6/mmm space group (no. 191), a=5.5835(9) Å, c=3.0278(6) Å).     

Use of vitamin B2 for fluorescence detection of thymidine-related single-nucleotide polymorphisms

In combination with abasic site (AP site)-containing DNAs, potential use of a biotic fluorescence compound, Vitamin B₂ (riboflavin), is demonstrated for the fluorescence detection of the thymine (T)-related single-nucleotide polymorphisms. Our method is based on construction of the AP site in DNA duplexes, which allows small ligands to bind to target nucleotides accompanied by fluorescence signaling: an AP site-containing probe DNA is hybridized with a target DNA so as to place the AP site toward a target nucleobase, by which hydrophobic microenvironments are provided for ligands to recognize target nucleotides through stacking and hydrogen-bonding interactions. In 10 mM sodium cacodylate buffer solutions (pH 7.0) containing 100 mM NaCl and 1.0 mM EDTA, Vitamin B₂ is found to selectively bind to T (K₁₁ = 1.8 × 10⁶ M⁻¹ at 5 °C) over other nucleobases, and this is accompanied by significant quenching of its fluorescence. While the sensing functions depend on the flanking sequences to the AP site, Vitamin B₂ is applicable to the detection of T/C (cytosine), T/G (guanine) and T/A (adenine) mutation sequences of the CYP2A6 gene, where the flanking nucleobases are guanines in both positions (-GXG-, X = AP site).     

K2B12F12: A rare A2X structure for an ionic compound at ambient conditions

The anhydrous salt K₂B₁₂F₁₂ crystallized from aqueous solution and its structure was determined by single crystal X-ray diffraction. The Ni₂In-type structure it exhibits is rare for an A₂X ionic compound at 25 °C and 1 atm., consisting of an expanded hexagonal close-packed array of B₁₂F₁₂²⁻ centroids (cent?cent distances: 7.204-8.236 Å) with half of the K⁺ ions filling all of the O_h holes and half of the K⁺ ions filling all of the D_3h trigonal holes in the close-packed layers that are midway between two “empty” T_d holes. The structure is also unusual in that the bond-valence sum for the K⁺ ions in O_h holes is less than or equal to 0.73 (the bond-valence sum for the other type of K⁺ ion is 1.16). A variation of the Ni₂In structure is exhibited by the previously published monohydrate Cs₂(H₂O)B₁₂F₁₂, for which an improved structure is also reported here. For K₂B₁₂F₁₂: monoclinic, C2/c, a = 8.2072(8), b = 14.2818(7), c = 11.3441(9) Å, β = 92.832(5)°, Z = 4, T = 120(2) K. For Cs₂(H₂O)B₁₂F₁₂: orthorhombic, P2₁2₁2₁, a = 9.7475(4), b = 10.2579(4), c = 15.0549(5) Å, Z = 4, T = 110(1) K.     

The study of Bi3B5O12: synthesis, crystal structure and thermal expansion of oxoborate Bi3B5O12

The paper presents a new data on the crystal structure, thermal expansion and IR spectra of Bi₃B₅O₁₂. The Bi₃B₅O₁₂ single crystals were grown from the melt of the same stoichiometry by Czochralski technique. The crystal structure of Bi₃B₅O₁₂ was refined in anisotropic approximation using single-crystal X-ray diffraction data. It is orthorhombic, Pnma, a=6.530(4), b=7.726(5), c=18.578(5) Å, V=937.2(5) Å³, Z=4, R=3.45%. Bi³⁺ atoms have irregular coordination polyhedra, Bi(1)O₆ (d(B-O)=2.09-2.75 Å) and Bi(2)O₇ (d(B-O)=2.108-2.804 Å). Taking into account the shortest bonds only, these polyhedra are considered here as trigonal Bi(1)O₃ (2.09-2.20 Å) and tetragonal Bi(2)O₄ (2.108-2.331 Å) irregular pyramids with Bi atoms in the tops of both pyramids. The BiO₄ polyhedra form zigzag chains along b-axis. These chains alternate with isolated anions [B₂^IVB₃^IIIO₁₁]⁷⁻ through the common oxygen atoms to form thick layers extended in ab plane. A perfect cleavage of the compound corresponds to these layers and an imperfect one is parallel to the Bi-O chains. The Bi₃B₅O₁₂ thermal expansion is sharply anisotropic (α₁₁≈α₂₂=12, α₃₃=3×10⁻⁶ °C⁻¹) likely due to a straightening of the flexible zigzag chains along b-axis and decreasing of their zigzag along c-axis. Thus the properties like cleavage and thermal expansion correlate to these chains.     

Iodination of cisplatin adduct of Vitamin B12 [{B12}-CN-{cis-PtCl(NH3)2}]

The cisplatin adduct of vitamin B₁₂, [{B₁₂}-CN-{cis-PtCl(NH₃)₂}]⁺ (1), reacts with iodide in aqueous solution to form [{B₁₂}-CN-{trans-PtI₂(NH₃)}] (3) in good yield. Mono-substitution of chloride was not observed since a subsequent replacement of one NH₃ by a second iodide is very fast as compared to the Cl⁻ → I⁻ exchange. The same reaction conditions allowed to introduce radioiodide ¹³¹I. Vitamin B₁₂ can therefore be labeled with radionuclides via binding to the Pt(II) center.     

Correlation between optical constants and crystal chemical parameters of ZrW2O8

The refractive indices of ZrW₂O₈, measured at wavelengths of 435.8-643.8 nm, were used to calculate n_D at λ=589.3 nm and n_∞ at λ=∞ from a one-term Sellmeier equation. Refractive indices, n_D and dispersion values, A, are, respectively, 1.8794 and 114×10⁻¹⁶ m². The high dispersion, relative to other molybdates, tungstates and Zr-containing compounds, is attributed to the low value of E_o=7.7 eV and mean cation coordination number. Total electronic polarizabilities, α_total, were calculated from n_∞ and the Lorenz-Lorentz equation. The unusually large difference between the observed polarizability of 20.087 Å³ and the calculated total polarizability α_T of 17.59 Å³ (Δ=+12.4%) is attributed to (1) a large M-O-W angle, (2) a high degree of W 5d-O_(terminal) 2p and Zr nd-O 2p hybridization, and (3) unusually high oxygen displacement factors, B(O), normalized to B(W).     

Interaction of polyhedral boron hydride anions [B10H10] and [B12H12] with cyclic copper and silver 3,5-bis(trifluoromethyl)pyrazolate complexes

The interactions of cyclic trinuclear copper {[3,5-(CF₃)₂Pz]Cu}₃ and silver {[3,5-(CF₃)₂Pz]Ag}₃ complexes with polyhedral borate anions [B₁₀H₁₀]²⁻ and [B₁₂H₁₂]²⁻ in solvents of low-polarity were studied using IR spectroscopy (190-290 K). Two types of complexes were found in solution: {[((3,5-CF₃)₂PzM)₃][B_nH_n]}²⁻ and {[((3,5-CF₃)₂PzM)₃]₂[B_nH_n]}²⁻ (M = Ag, Cu; n = 10, 12). The stability constants of these complexes were determined from IR-spectra.     

Dipstick based immunochemiluminescence biosensor for the analysis of vitamin B12 in energy drinks: A novel approach

In this article, we describe a dipstick based immunochemiluminescence (immuno-CL) biosensor for the detection of vitamin B₁₂ in energy drinks. The method is a direct competitive type format involving the immobilization of vitamin B₁₂ antibody on nitrocellulose membrane (NC) followed by treatment with vitamin B₁₂ and vitamin B₁₂–alkaline phosphatase conjugate to facilitate the competitive binding. The dipstick was further treated with substrate disodium 2-chloro-5-(4-methoxyspiro {1,2-dioxetane-3,2¢-(5¢-chloro)tricyclo[3.3.1.13,7]decan}-4-yl)-1-phenyl phosphate (CDP-Star) to generate chemiluminescence (CL). The number of photons generated was inversely proportional to the vitamin B₁₂ concentration. After systematic optimization, the limit of detection was 1 ng mL⁻¹. The coefficient of variation was below 0.2% for both intra- and inter-assay precision. Vitamin B₁₂ was extracted from energy drinks with recovery ranged from 90 to 99.4%. Two different energy drinks samples were analyzed, and a good correlation was observed when the data were compared with a reference enzyme linked immuno sorbent assay (ELISA) method. The developed method is suitable for an accurate, sensitive, and high-throughput screening of vitamin B₁₂ in energy drinks samples. The dipstick technique based on immuno-CL is suitable for the detection of several analyte in food and environmental samples.     

Decomposition of tetraalkylammonium thiotungstates characterized by thermoanalysis, mass spectrometry, X-ray diffractometry and scanning electron microscopy

Thermal decomposition reactions of tetraalkylammonium thiotungstates, (R₄N)₂WS₄ (R = methyl to heptyl), were investigated with DSC and DTA-TG coupled with mass spectroscopy (MS). The results demonstrate that the complexity of thermal decomposition reactions is significantly influenced by the alkyl group, i.e., more complex steps are observed for the materials with longer alkyl chain lengths. Tetraethyl and tetrapropyl complexes show reversible and irreversible phase transitions detected by DSC experiments combined with thermodiffractometry. The tetrapentyl compound undergoes an irreversible phase transition while the tetraheptyl sample exhibits a glass-like transition and melting prior to decomposition. The whole series of compounds decompose without forming sulfur rich WS_n (n = 3 or 4) intermediates. The final WS₂ products are nearly stoichiometric for R = methyl to pentyl but for hexyl and heptyl samples the sulfur content is significantly reduced with a W/S ratio of about 1.5. The residual carbon and hydrogen contents increase in the final decomposition products in the same order as the number of C atoms in R₄N increase. For the N content no clear trend is obvious. A general thermal decomposition mechanism is suggested which follows a bimolecular nucleophilic substitution reaction. In the SEM images only for R = heptyl the formation of macro-pores with a sponge-like morphology is seen, but for the other precursors compact materials are formed which in part display a well developed morphology. X-ray diffraction analysis of the final products shows the formation of amorphous WS₂ up to the tetrapentyl precursor. But for the tetrahexyl and tetraheptyl materials the W:S ratio is significantly smaller than 1:2 and large amounts of C and H are determined by chemical analyses. In accordance with previously reported results it can be assumed that a carbosulfide phase is formed by a mixed C-W-S sandwich layered structure.     

Order-disorder at Fe sites in SrFe2/3B″1/3O3 (B″=Mo, W, Te, U) tetragonal double perovskites

We have prepared SrFe_2/3B″_1/3O₃ (B″=Mo, U, Te, and W) double perovskites in polycrystalline form by ceramic methods. Phases with B″=U, Te and W have been studied by X-ray powder diffraction and the results have been compared with neutron diffraction data available for B″=Mo. At room temperature, the stoichiometric samples crystallize in the tetragonal crystal system (space group I4/m, Z=4). Cell parameters when B″=U, Te and W are a=5.6936(1) Å, c=8.0637(1)Å; a=5.5776(1) Å, c=7.9144(3) Å and a=5.5707(3) Å, c=7.9081(5) Å, respectively.The Mössbauer spectra at room temperature for all compounds show hyperfine parameters belonging to two Fe³⁺ sites located at lattice positions with different degrees of distortion. This is in agreement with diffraction data that indicate that the series of compounds display different degrees of Fe-site disorder, which increases in the following sequence: Mo<U<Te<W.     

New synthesis and thermal studies of palladacycloalkanes and their precursors

A series of new palladacycloalkanes of formula cis-[PdL₂(CH₂)_n] (9. n = 6, L = PPh₃; 10. n = 6, L₂ = dppe; 11. n = 8, L = PPh₃; 12. n = 8, L₂ = dppe) have been prepared by two routes. In the first route, the precursor bis(1-alkenyl) complexes cis-[PdL₂((CH₂)_nCHCH₂)₂] (1. n = 2, L = PPh₃, 2. n = 2, L₂ = dppe, 3. n = 3, L = PPh₃, 4. n = 3, L₂ = dppe) were allowed to react with Grubb’s 2nd generation catalyst to give the palladacycloalkenes, cis-[PdL₂(CH₂)_nCHCH(CH₂)_n] (5. n = 2, L = PPh₃, 6. n = 2, L₂ = dppe, 7. n = 3, L = PPh₃, 8. n = 3, L₂ = dppe), which were then hydrogenated to the palladacycloalkanes, 9-12. In the second route, the di-Grignard reagents BrMg(CH₂)_nMgBr (n = 6, 8) were reacted with the palladium complex [PdCl₂(COD)] followed by immediate ligand displacement to form the respective palladacycloalkanes 10 and 12. The complexes obtained were characterized by a range of spectroscopic and analytical techniques. Thermal decomposition studies were carried out on the palladacycloalkanes 9-12 and the main organic products shown to be 1-alkenes and 2-alkenes.     

A validated stripping voltammetric procedure for quantification of the anti-hypertensive and benign prostatic hyperplasia drug terazosin in tablets and human serum

The electrochemical behavior of terazosin at the hanging mercury drop electrode was studied in Britton-Robinson buffer (pH 2-11), acetate buffer (4.5-5.5), and in 0.1 M solution of each of sodium sulfate, sodium nitrate, sodium perchlorate and potassium chloride as supporting electrolytes. The square-wave adsorptive cathodic stripping voltammogram of terazosin exhibited a single well-defined two-electron irreversible cathodic peak which may be attributed to the reduction of CO double bond of the drug molecule. A fully validated, simple, high sensitive, precise and inexpensive square-wave adsorptive cathodic stripping voltammetric procedure was described for determination of terazosin in bulk form, tablets and human serum. A mean recovery for 1×10⁻⁸ M terazosin in bulk form, following preconcentration onto the hanging mercury drop electrode for 60 s at a −1.0 V (versus Ag/AgCl/KCl_s), of 99±0.7% (n=5) was obtained. Limits of detection (LOD) and quantitation (LOQ) of 1.5×10⁻¹¹ and 5×10⁻¹¹ M bulk terazosin were achieved, respectively. The proposed procedure was successfully applied to determination of the drug in its Itrin^® tablets and human serum samples. The achieved LOD and LOQ of the drug in human serum samples were 5.3×10⁻¹¹ and 1.8×10⁻¹⁰ M THD, respectively. The pharmacokinetic parameters of the drug in human plasma were estimated as: C_max=77.5 ng ml⁻¹, t_max=1.75 h, AUC_0-t=602.3 ng h ml⁻¹, K_e=0.088 h⁻¹ and t_1/2=11.32 h) which are favorably compared with those reported in literature.     

Validated liquid chromatography method for assay of tizanidine in drug substance and formulated products

A new isocratic stability indicating HPLC method for determination of tizanidine in drug substance and formulated products is described. Chromatographic separation of tizanidine from the related substances and degraded products was achieved with a Hypersil CN column ( mm, 5 μm) using a mobile phase comprising a mixture of an ion-pairing solution of heptanesulphonic acid sodium salt (HAS), methanol and acetonitrile (50:57:18 (v/v)) within 10 min. The flow-rate was 1.0 ml/min and detection was made at 227 nm. The method has good selectivity towards tizanidine, related substances and degraded products. Limits of quantitation for tizanidine and its synthetic intermediates were determined, ranging from 0.051 to 0.54 μg/ml. The linearity range was found to be 2-20 μg/ml (r=0.9998, n=5). Mean recovery for tizanidine from the tablets was from 99.5 to 99.8%. Precision of the method was 1.0% (n=9). The method can be used for routine analysis and the quality control of tizanidine drug substance and its formulated products.     

Synthesis, structure characterization and optical properties of a new tripotassium cadmium pentaborate, K3CdB5O10

A new ternary borate oxide, K₃CdB₅O₁₀, has been synthesized by solid-state reaction at 580 °C. The compound crystallizes in the monoclinic space group P2₁/n with a=7.6707 (7) Å, b=19.1765 (17) Å, c=7.8784 (6) Å, β=115.6083 (49)°, and Z=4. The crystal structure consists of a two-dimensional infinite [CdB₅O₁₀] layer, which forms by connecting isolated double ring [B₅O₁₀] groups and CdO₄ tetrahedra. K atoms filling in the interlayer and intralayer link the layers together and balance charge. The IR spectrum has been studied and confirmed the presence of both BO₃ and BO₄ groups, and the UV-vis-IR diffuse reflectance spectrum exhibits a band gap of about 3.4 eV. The DSC analysis proves that K₃CdB₅O₁₀ is a congruent melting compound.     

A correlation study of bisphosphine ligand bite angles with enantioselectivity in Pd-catalyzed asymmetric transformations

Among the bisphosphine ligands, we have previously developed C_n-TunePhos (n = 1-6) as a family of ligands with tunable bite angles. The increase in spacer -CH₂- groups in this family of ligands causes changes in ligand dihedral angle, which in turn causes P-Pd-P bite angle variation. Pd-catalyzed asymmetric alkylations and cycloadditions have been tested with C_n-TunePhos ligands. This study aims at a possible correlation between ligand bite angles with enantioselectivity of the Pd-catalyzed asymmetric products.     

Fluorescence resonance energy transfer between acridine orange and rhodamine 6G and its analytical application for vitamin B12 with flow-injection laser-induced fluorescence detection

By coupling flow-injection with laser-induced fluorescence detection, a setup was developed and a novel method combining fluorescence resonance energy transfer (FRET) and flow-injection analysis (FIA) was proposed for the determination of vitamin B₁₂ (VB₁₂) based on its fluorescence quenching on the system of acridine orange (AO)/rhodamine 6G (R6G). The effective energy transfer could occur between AO and R6G in the dodecyl benzene sodium sulfonate (DBS) while 454 nm argon laser was used as the excitation source, and as a result, the fluorescence emission of R6G has been increased significantly. It was found that the fluorescence of the above system could be sharply diminished by VB₁₂. By using the mixed solution AO-R6G-DBS and the same solution containing VB₁₂ as the carrier and sample, respectively, a series of negative peaks which could be applied for the quantification of VB₁₂ were obtained. The detection limit for VB₁₂ was 1.65 × 10⁻⁶ mol/L. The linear range for determining VB₁₂ was 4 × 10⁻⁴ to 2 × 10⁻⁶ mol/L (correlation coefficient, r = 0.9923). The method was applied to measure VB₁₂ injections with satisfactory results.     

Crystal growth and structural investigation of A2BReO6 (A=Sr, Ba; B=Li, Na)

Single crystals of the double perovskite rhenates A₂BReO₆ (A=Sr, Ba; B=Li, Na) were grown out of molten hydroxide fluxes. Single crystals of orange/yellow Ba₂LiReO₆, Ba₂NaReO₆ and Sr₂LiReO₆ were solved in the cubic, Fm-3m space group with a=8.1214(11) Å, 8.2975(3) Å, and 7.9071(15) Å, respectively, while Sr₂NaReO₆ was determined to be monoclinic P2₁/n with a=5.6737(6) Å, b=5.7988(6) Å, c=8.0431(8) Å, and β=90.02(6) °. The cubic structure consists of a rock salt lattice of corner-shared ReO₆ and MO₆ (M=Li, Na) octahedra which, in the monoclinic structure, are both tilted and rotated. A discrepancy exists between the symmetry of Sr₂LiReO₆ indicated by the single-crystal refinement of flux-grown crystals (cubic, Fm-3m) and the symmetry indicated by the powder diffraction data collected on polycrystalline samples prepared by the ceramic method (tetragonal, I4/m). It is possible that the cubic crystals are a kinetic product that forms in small quantities at low temperatures, while the powder represents the more stable polymorph that forms at higher reaction temperature.     

The non-centrosymmetric borate oxides, MBi2B2O7 (M=Ca, Sr)

Two novel noncentrosymmetric borates oxides, MBi₂B₂O₇ or MBi₂O(BO₃)₂ (MCa, Sr), have been synthesized by solid-state reactions in air at temperatures in the 600-700 °C range. Their crystal structures have been determined ab initio and refined using powder neutron diffraction data. CaBi₂B₂O₇ crystallizes in the orthorhombic Pna2₁ space group with a=8.9371(5) Å, b=5.4771(3) Å, c=12.5912(7) Å, Z=4, R_wp=0.118, χ²=2.30. SrBi₂B₂O₇ crystallizes in the hexagonal P6₃ space group with a=9.1404(4) Å, c=13.0808(6) Å, Z=6, R_wp=0.115, χ²=4.15. Large displacement parameters suggest the presence of disorder in SrBi₂B₂O₇ as also revealed by diffuse 2×a superstructure reflections in electron diffraction patterns. Both structures are built of identical (001) neutral layers of corner-sharing BO₃ triangles and MO₆ trigonal prisms forming six-membered rings in which Bi₂O groups are located. Adjacent layers are stacked in a staggered configuration and connected through weak Bi-O bonds. A moderate efficiency for second harmonic generation (SHG) has been measured for a powder sample of CaBi₂B₂O₇ (d_eff=2d_eff(KDP)).     

On phase equilibria and crystal structures in the systems Ce-Pd-B and Yb-Pd-B. Physical properties of R2Pd13.6B5 (R=Yb, Lu)

Phase equilibria and crystal structures of ternary compounds were determined in the systems Ce-Pd-B and Yb-Pd-B at 850 °C in the concentration ranges up to 45 and 33 at% of Ce and Yb, respectively, employing X-ray single crystal and powder diffraction. Phase relations in the Ce-Pd-B system at 850 °C are governed by formation of extended homogeneity fields, τ₂-CePd₈B_2−x (0.10<x<0.48); τ₃-Ce₃Pd_25−xB_8−y (1.06<x<1.87; 2.20<y<0.05), and CePd₃B_x (0<x<0.65) the latter arising from binary CePd₃. Crystallographic parameters for the new structure type τ₂-CePd₈B_2−x (space group C2/c, a=1.78104(4) nm, b=1.03723(3) nm, c=1.16314(3), β=118.515(1)° for x=0.46) were established from X-ray single crystal diffraction. The crystal structures of τ₂-CePd₈B_2−x and τ₃-Ce₃Pd_25−xB_3−y are connected in a crystallographic group-subgroup relationship. Due to the lack of suitable single crystals, the novel structure of τ₁-Ce₆Pd_47−xB₆ (x=0.2, C2/m space group, a=1.03594(2) nm, b=1.80782(3) nm, c=1.01997(2) nm, β=108.321(1)°) was determined from Rietveld refinement of X-ray powder diffraction data applying the structural model obtained from single crystals of homologous La₆Pd_47−xB₆ (x=0.19) (X-ray single crystal diffraction, new structure type, space group C2/m, a=1.03988(2) nm, b=1.81941(5) nm, c=1.02418(2) nm, β=108.168(1)°).The Yb-Pd-B system is characterized by one ternary compound, τ₁-Yb₂Pd₁₄B₅, forming equilibria with extended solution YbPd₃B_x, YbB₆, Pd₅B₂ and Pd₃B. The crystal structures of both Yb₂Pd₁₄B₅ and isotypic Lu₂Pd₁₄B₅ were determined from X-ray Rietveld refinements and found to be closely related to the Y₂Pd₁₄B₅-type (I4₁/amd). The crystal structure of binary Yb₅Pd_2−x (Mn₅C₂-type) was confirmed from X-ray single crystal data and a slight defect on the Pd site (x=0.06) was established.The three structures τ₁-Ce₆Pd_47−xB₆, τ₂-CePd₈B_2−x and τ₃-Ce₃Pd_25−xB_8−y are related and can be considered as the packings of fragments observed in Nd₂Fe₁₄B structure with different stacking of common structural blocks.Physical properties for Yb₂Pd_13.6B₅ (temperature dependent specific heat, electrical resistivity and magnetization) yielded a predominantly Yb-4f¹³ electronic configuration, presumably related with a magnetic instability below 2 K. Kondo interaction and crystalline electric field effects control the paramagnetic temperature domain.