Zur Kenntnis der Chemie der Silazane. IV. Über ein Sulfurylphosphazo-silazan

Trichlorophosphazo-sulphurylchloride. Cl₃P?N? SO₂Cl, reacts with heptamethyldisilazane to yield the Si? N? P compound (I) formulated in ?Inhaltsübersicht”?. (I) reacts with PCl₅ or C₆H₅? PCl₄ forming the known 2,2,2,4,4,4-hexachloro-1,3-di-methylcyclo-diphosphazane(II), accompanied by the compound Cl₃P?N? SO₂Cl and C₆H₅? PCl₂?N? SO₂Cl, respectively, which were detected by means of ³¹P-NMR spectroscopy.     

Aminophosphane. XI. Einige Reaktionen des N-Diphenylphosphino-triphenyl-phosphazens

N-Diphenylphosphino-triphenylphosphazene possesses a highly reactive (C₆H₅)₂P group. At room temperature CH₃J adds to give (C₆H₅)₃P?N?P(C₆H₅)₂CH ₃J whilst phenylbromide did not react under similar conditions. The phosphorous halides (C₆H₅)₂PX(X = Cl, Br)add in a 1:1 mole ratio to yield (C₆H₅)₃P?N?P(C₆H₅)₂? PC₆H₅)₂X; this addition is also the preferred reaction with C₆H₅PCl₂, but PCl₃ is in part dehalogenated by (C₆H₅)₃P?N? P(C₆H₅)₂, and PSCl₃ desulfurized. The chalcogens O, S, Se, Te readily add to the P(III) atom of the base and this is also the case with BH₃. CS₂ forms the betaine (C₆H₅)₃ · · P?N? P(C₆H₅)₂? C(S)S. The IR and NMR spectra of the new compounds are discussed.     

Über Phosphorstickstoffverbindungen. XXXIII. Reaktionen von Diphenyltrichlorphosphoran mit Hydraziniumsalzen und -derivaten

Hydrazinium monochloride disproportionates on interaction with diphenyl-trichlorophosphorane, giving N₂ and [(C₆H₅)₂P(Cl)? N? PCl(C₆H₅)₂]Cl. The phosphinazine dihydrochloride [(C₆H₅)₂PCl? NH? NH? PCl(C₆H₅)₂]Cl₂ is obtained according to equation (4). The preparation of the P? N five-ring compound X, formulated in ?Inhaltsübersicht”?, is described.     

Luminescent Amphiphilic 2,6‐Bis(1‐alkylpyrazol‐3‐yl)pyridyl Platinum(II) Complexes: Synthesis,Characterization, Electrochemical,Photophysical, and Langmuir–Blodgett Film Formation Studies

Two series of novel platinum(II) 2,6‐bis(1‐alkylpyrazol‐3‐yl)pyridyl (N5Cn) complexes, [Pt(N5Cn)Cl][X] ( 1 – 9 ) and [Pt(N5Cn)(C?CR)][X] ( 10 – 13 ) (X=trifluoromethanesulfonate (OTf) or PF₆; R=C₆H₅, C₆H₄‐p‐CF₃ and C₆H₄‐p‐N(C₆H₅)₂), with various chain lengths of the alkyl groups on the nitrogen atom of the pyrazolyl units have been successfully synthesized and characterized. Their electrochemical and photophysical properties have been studied. Some of their molecular structures have also been determined by X‐ray crystallography. Two amphiphilic platinum(II) 2,6‐bis(1‐tetradecylpyrazol‐3‐yl)pyridyl (N5C14) complexes, [Pt(N5C14)Cl]PF₆ ( 7 ) and [Pt(N5C14)(C?CC₆H₅)]PF₆ ( 13 ), were found to form stable and reproducible Langmuir–Blodgett (LB) films at the air–water interface. The characterization of such LB films has been investigated by the study of their surface pressure–area (π–A) isotherms, UV/Vis spectroscopy, XRD, X‐ray photoelectron spectroscopy (XPS), FTIR, and polarized IR spectroscopy. The luminescence property of 13 in LB films has also been studied.     

Thermal properties of N-substituted 4-vinylpyridinium ions and their polymers

4-Vinylpyridinium trifluoromethanesulfonate monomers substituted at nitrogen with H, O, CH₃, C₂H₅, C₆H₁₃, and C₁₂H₂₅ were synthesized and characterized spectroscopically. Thermal analyses (DSC and TGA) were carried out on all the compounds. The solid monomers (N? H, N? CH₃, N? C₆H₁₃, and N? C₁₂H₂₅) exhibited endothermic melting followed by exothermic polymerization and exothermic decomposition (>400°C). Liquid N? C₂H₅ monomer revealed only exothermic polymerization and decomposition. The N? O polymer underwent thermal decomposition below 300°C. The N–C₁₂H₂₅ homopolymer, prepared from monomer in the DSC or in bulk, displayed an unusual thermal transition at 250°C, which has been attributed to a polymer backbone reorientation leading to side-chain ordering of the dodecyl groups.     

Darstellung und Kristallstruktur von [P(C6H5)4][2,9-{N,N′-(2-NH?(C5H4N))}B10H8]

Synthesis and Crystal Structure of [P(C₆H₅)₄][2,9-{N,N′-(2-NH? (C₅H₄N))}B₁₀H₈] [N(C₄H₉)₄]₂[B₁₀H₁₀] reacts with 2-aminopyridine forming a product mixture from which [2,9-{N,N′-(2-NH? (C₅H₄N))}B₁₀H₈]^? can be isolated by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose. The crystal structure of [P(C₆H₅)₄][2,9-{N,N′-(2-NH? (C₅H₄N))}B₁₀H₈] (triclinic, space group P1 , a = 10.1103(9), b = 11.5665(9), c = 14.877(2) Å, α = 102.600(8), β = 107.567(8) und γ = 96.487(7)°, Z = 2) reveals the bonding of 2-NH₂-(C₅H₄N) via both N atoms to vicinal B atoms of the two square planes of the B₁₀ cluster (B2? N1 = 1,541(7) und B9? N2 = 1.505(7) Å) forming a five-membered ring.     

Polysulfonylamine. XLVI Molekülkomplexe von Di(organosulfonyl)aminen mit Dimethylsulfoxid und Triphenylphosphinoxid. Röntgenstrukturanalyse von Di(4-fluorbenzolsulfonyl)amin-Dimethylsulfoxid(2/1)

Polysulfonyl Amines. XLVI. Molecular Adducts of Di(organosulfonyl)amines with Dimethyl Sulfoxide and Triphenylphosphine Oxide. X-Ray Structure Determination of Di(4-fluorobenzenesulfonyl)amine-Dimethyl Sulfoxide(2/1) From equimolar solutions of the respective components in CH₂Cl₂/petroleum ether, the following crystalline addition compounds were obtained: (X? C₆H₄SO₂)₂NH …? OS(CH₃)₂, where X = H, 4? CH₃, 4? Cl, 4? Br, 4? I, 4? NO₂ or 3? NO₂; [(4? F? C₆H₄SO₂)₂NH]₂ · (OS(CH)₃)₂ ( 8 ); (4? I? C₆H₄SO₂)₂NH · OP(C₆H₅)₃. A (2/1) complex of (4? F? C₆H₄SO₂)₂NH with OP(C₆H₅)₃ could not be isolated. The solid-state structure of the (2/1) compound 8 is compared with the known structure of the (1/1) complex (CH₃SO₂)₂NH · OS(CH₃)₂. The crystallographic data for 8 at ?95°C are: monoclinic, space group C2/c, a = 2 369.9(13), b = 1 006.8(4), c = 2 772.6(13) pm, β = 110.71(4)°, U = 6.187 nm³, Z = 8. Two N? H …? O hydrogen bonds with N …? O 275 and 280 pm connect the disulfonylamine molecules with the dimethyl sulfoxide molecule. The O atom of the latter has a trigonal-planar environment consisting of the S atom and the two hydrogen bond H atoms.     

Luminescent Amphiphilic 2,6‐Bis(1,2,3‐triazol‐4‐yl)pyridine?Platinum(II) Complexes: Synthesis,Characterization, Electrochemical,Photophysical, and Langmuir–Blodgett Film‐Formation Studies

A new series of platinum(II) complexes with tridentate ligands 2,6‐bis(1‐alkyl‐1,2,3‐triazol‐4‐yl)pyridine and 2,6‐bis(1‐aryl‐1,2,3‐triazol‐4‐yl)pyridine (N7R), [Pt(N7R)Cl]X ( 1 – 7 ) and [Pt(N7R)(C?CR′)]X ( 8 – 17 ; R=n‐C₄H₉, n‐C₈H₁₇, n‐C₁₂H₂₅, n‐C₁₄H₂₉, n‐C₁₈H₃₇, C₆H₅, and CH₂‐C₆H₅; R′=C₆H₅, C₆H₄‐CH₃‐p_, C₆H₄‐CF₃‐p, C₆H₄‐N(CH₃)₂‐p, and cholesteryl 2‐propyn‐1‐yl carbonate; X=OTf^?, PF₆^?, and Cl^?), has been synthesized and characterized. Their electrochemical and photophysical properties have also been studied. Two amphiphilic platinum(II)? 2,6‐bis(1‐dodecyl‐1,2,3‐triazol‐4‐yl)pyridine complexes ( 3‐Cl and 8 ) were found to form stable and reproducible Langmuir–Blodgett (LB) films at the air/water interface. These LB films were characterized by the study of their surface‐pressure–molecular‐area (π–A) isotherms, XRD, and IR and polarized‐IR spectroscopy.     

Synthesis and structures of the six-coordinate donor-acceptor complexes R3(C6H4O2)Sb…L (R=Ph, L=OSMe2 or ONC5H5; R=Me, L=ONC5H5 or NC5H5) and R3(C2H4O2)Sb…L (R=Ph, L=ONC5H5; R=Cl or C6F5, L=OPPh3)

One-pot oxidation of R₃Sb (R=Ph, Me, Cl, or C₆F₅) withtert-butyl hydroperoxide in the presence of 1,2-diols and monodentate donor compounds was studied. The structures of the resulting neutral organic donor-acceptor Sb^V complexes, Ph₃(C₆H₄O₂)Sb…OSMe₂, Ph₃(C₆H₄O₂)Sb…ONC₅H₅, Me₃(C₆H₄O₂)Sb…ONC₅H₅, Me₃(C₆H₄O₂)Sb…NC₅H₅, Ph₃(C₂H₄O₂)Sb…ONC₅H₅, and Cl(C₆F₅)₂(C₂H₄O₂)Sb…OPPh₃, were established by X-ray diffraction analysis. In these complexes, the coordination environment about the Sb atoms is a distorted octahedron. The Sb?O(N) distances and the Sb?O?E angles (E=S, N, or P) vary over wide ranges.     

Untersuchungen über das Reaktionsverhalten von Antimonpentachlorid. III [1]. Zur Reaktion von Antimon (V)-chlorid mit Methylisocyanat

Studies on the Reactivity of Antimony Pentachloride. III. The Reaction of Antimony(V) Chloride and Methylisocyanate Methylisocyanate CH₃NCO reacts with SbCl₅ in boiling CCl₄ by an insertion-reaction to a product of the formula C₅H₆Cl₉N₂O₂Sb I, which has the chlorformamidinium-structure (Cl? C(O)? N(CH₃)? CCl? N(CH₃)? C(O)? Cl)⊕SbCl₆?. Hydrolysis of I yields the heterocycle C₅H₆N₂O₄ II. The reaction with methanol gives (CH₃? NH? CCl? NH? CH₃)⊕SbCl₆? III and (CH₃? NH? CCl? N(CH₃)? C(O)? OCH₃)⊕SbCl₆? IV. The i.r. and Raman spectra of the compounds I, III and IV are discussed.     

Synthesis,Interionic Structure,and Reactivity toward CO and p‐Methylstyrene of Palladacyclic Compounds Bearing α‐Diimine Ligands

Palladacyclic compounds [Pd(C₆H₄(C₆H₅C?O)C?N? R)(N? N)] [X] (R = Et, ⁱPr, 2,6‐ⁱPr₂C₆H₃; N? N = bpy = 2,2′‐bipyridine, or 1,4‐(o,o′‐dialkylaryl)‐1,4‐diazabuta‐1,3‐dienes; [X]^? = [BF₄]^? or [PF₆]^?) were synthesized from the dimers [{Pd(C₆H₄(C₆H₅C?O)C?N? R)(μ‐Cl)}₂] and N? N ligands. Their interionic structure in CD₂Cl₂ was determined by means of ¹⁹F,¹H‐HOESY experiments and compared with that in the solid state derived from X‐ray single‐crystal studies. [Pd(C₆H₄(C₆H₅C?O)C?N? R)(N? N)] [X] complexes were found to copolymerize CO and p‐methylstyrene affording syndiotactic or isotactic copolymers when bpy or 1,4‐(o,o′‐dimethylaryl)‐1,4‐diazabuta‐1,3‐dienes were used, respectively. The reactions with CO and p‐methylstyrene of the bpy derivatives were investigated. Two intermediates derived from a single and a double insertion of CO into the Pd? C bonds were isolated and completely characterized in solution.     

Über Chalkogenolate. 127. Diester der Cyaniminodiameisensäure NC?N(CO?OR)2 mit R = CH3, C2H5 und C6H5. Thiolyse der Diester

On Chalcogenolates. 127. Diesters of Cyanimino Diformic Acid NC? N(CO? OR)₂, where R = CH₃, C₂H₅, and C₆H₅. Thiolysis of these Diesters The diesters NC? N(CO? OR)₂ have been prepared by reaction of the sodium salt of cyanamide with the corresponding chloroformic acid ester. The thiolysis of these esters yields H₂N? CS? NH? CO? OR. The compounds with R = CH₃, C₂H₅, and C₆H₅ have been characterized by means of diverse methods.     

New Dinuclear Ru2(CO)4 Sawhorse‐Type Complexes Containing Bridging Carboxylato Ligands

The thermal reaction of Ru₃(CO)₁₂ with ethacrynic acid, 4‐[bis(2‐chlorethyl)amino]benzenebutanoic acid (chlorambucil), or 4‐phenylbutyric acid in refluxing solvents, followed by addition of two‐electron donor ligands (L), gives the diruthenium complexes Ru₂(CO)₄(O₂CR)₂L₂ ( 1 : R = CH₂O‐C₆H₂Cl₂‐COC(CH₂)C₂H₅, L = C₅H₅N; 2 : R = CH₂O‐C₆H₂Cl₂‐COC(CH₂)C₂H₅, L = PPh₃; 3 : R = C₃H₆‐C₆H₄‐N(C₂H₄‐Cl)₂, L = C₅H₅N; 4 : R = C₃H₆‐C₆H₄‐N(C₂H₄‐Cl)₂, L = PPh₃; 5 : R = C₃H₆‐C₆H₅, L = C₅H₅N; 6 : R = C₃H₆‐C₆H₅, L = PPh₃). The single‐crystal structure analyses of 2 , 3 , 5 and 6 reveal a dinuclear Ru₂(CO)₄ sawhorse structure, the diruthenium backbone being bridged by the carboxylato ligands, while the two L ligands occupy the axial positions of the diruthenium unit.     

Kristallstruktur von Dipyridiniomethan-Monohalogenohydro-closo-Decaboraten(2–), [(C5H5N)2CH2][2-XB10H9]; X  Cl,Br, I

Crystal Structures of Dipyridiniomethane Monohalogenohydro-closo-Decaborates(2–), [(C₅H₅N)₂CH₂][2-XB₁₀H₉]; X = Cl, Br, I [B₁₀H₁₀]^2? reacts with chlorine, bromine and iodine or with N-halogenosuccinimide, yielding the monohalogenodecaborates [2-XB₁₀H₉]^2? (X = Cl, Br, I), which are separated by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose from the starting compound and higher halogenated products. The X-ray structure determinations of the isotypic chloro and bromo compounds [(C₅H₅N)₂CH₂][2-XB₁₀H₉] (monoclinic, space group C2/c, Z = 8; for X ? Cl: a = 33.174(5), b = 7.2809(4), c = 16.2232(7) Å, β = 113.307(7)°; for X = Br: a = 33.525(11), b = 7.281(2), c = 16.297(4) Å, β = 113.62(2)°) and of the iodo compound [(C₅H₅N)₂CH₂][2-IB₁₀H₉] (monoclinic, space group P2₁, Z = 2, a = 7.143(3), b = 13.568(4), c = 9.479(7) Å, β = 97.57(5)°) show columns of substituted boron clusters [2-XB₁₀H₉]^2?, X = Cl, Br, I and bent dications [(C₅H₅N)₂CH₂]²⁺ along the shortest axis wich are assembled to alternating layers in the crystal lattice.     

Synthesis,structural characterization,and in vitro antimicrobial properties of salicylate and pyrazoline complexes of bismuth(III)

Displacement reactions of dichlorobismuth(III)pyrazolinates with oxygen donors such as sodium salicylate and acetate in 1?:?1 and 1?:?2 molar ratio in refluxing anhydrous benzene yields (C₁₂H₁₅N₂OX)Bi(C₆H₄O₃), (CH₃COO)BiCl(C₁₅H₁₂N₂OX), and (CH₃COO)₂Bi(C₁₅H₁₂N₂OX) [C₁₂H₁₅N₂OX?=?3(2′-hydroxyphenyl)-5-(4-X-substituted phenyl) pyrazoline X?=?H in 1,5,9, CH₃ in 2,6,10, OCH₃ in 3,7,11, and Cl in 4,8,12, respectively, (C₆H₄O₃)?=?salicylate and (CH₃COO)?=?acetate]. Newly synthesized derivatives are brown solids, soluble in organic solvents like benzene, chloroform, and acetone. The compounds have been characterized by elemental analyses (C, H, N, Cl, and Bi), molecular weight measurements, and spectral (IR, ¹H NMR, ¹³C NMR) studies. The (C₁₂H₁₅N₂OX) and (C₆H₄O₃) are bidentate while (CH₃COO) is monodentate to bismuth(III), leading to a distorted trigonal bipyramidal structure. The complexes were screened against different bacteria and fungi showing potential antibacterial and antifungal activities.     

Ferrocene­carboxyl­ic acid–1,4‐di­aza­bi­cyclo­[2.2.2]­octane (2/1): sheets built from O—H⃛N and C—H⃛O hydrogen bonds

In the title compound, 2[Fe(C₅H₅)(C₆H₅O₂)]·C₆H₁₂N₂, the molecular components are linked into finite three‐component aggregates by strong O—H?N hydrogen bonds [O?N 2.578 (4) and 2.604 (5) Å; O—H?N 170 (5) and 174 (6)°]; these aggregates are further linked by C—H?O hydrogen bonds [C?O 3.327 (5)–3.401 (5) Å; C—H?O 149–157°] into continuous sheets in the form of (6,3) nets.     

Spektroskopische Untersuchungen an Siliciumverbindungen. XXXI. Schwingungsverhalten von p-substituierten N,N-Bistrimethylsilylanilinen

The following p-substituted N,N-bis-trimethlsilyl anilines p-X? C₆H₄? N[Si(CH₃)₃]₂ are prepared by silylation of free amines: X = H, CH₃, C₂H₅, CH₃O, CH₃CO, F, Cl, Br, J, CN, C₆H_S, (CH₃)₃SiO, and [(CH₃)₃Si]₂N, and the isotopic derivatives C₆H₅? ¹⁵N[Si(CH₃)₃]₂ and C₆D₅N[Si(CH₃)₃]₂. The vibrational spectra are reported and assigned. The molecular symmetry of p-[(CH₃)₃Si]₂N? C₆H₄? N[Si(CH₃)₃]₂ is determined. The influence of the mass of the substituents X on the positions of the ν_sSiNSi vibrational frequencies is discussed.     

Die Elektronenstoßfragmentierung von substituierten Dimethylalkoxysilanen

Electron Impact Fragmentation of Substituted Dimethylalkoxysilanes The mass spectra of substitued dimethylalkoxysilanes (H₃C)₂SiOCH₃R (R ? ? F, ? Cl, ? H, ? OCH₃, ? C₆H₅, ? CH₃, ? C₂H₅, ? n-C₃H₇), and (H₃C)₂SiOC₂H₅R (R ? ? Cl, ? C₆H₅, ? CH₃, ? C₂H₅) have been recorded and the fragmentation patterns are presented. The yield of the electron impact induced reaction (M-15)⁺→(M-45)⁺+ H₂CO occuring upon fragmentation of substituted dimethylmethoxysilanes depends on the substituent R. A quantum chemical calculation was carried out by CNDO/2 method to determine the electron density distribution in the ion at mass number (M-15). It is shown that a correlation exists between the Si? O? π bond order in this ion and the yield as well as the activation energy of this reaction.     

Untersuchungen an Selen-Verbindungen. LXIX. Über das Reaktionsverhalten von Diphenylselendihalogeniden mit Ammoniak,Alkyl- und Silylaminen

Studies on Selenium Compounds. LXIX. On the Reactivity of Diphenyl Selenium Dihalides with Ammonia, Alkyl- and Silylamines The halides Ph₂SeX₂ (Ph = C₆H₅; X = Cl, Br) are reduced by NH₃, MeNH₂ and Me₂NH (Me = CH₃) at ?60°C forming Ph₂Se. The reaction of Ph₂SeCl₂ with Me₃SiNMe₂ yields Ph₂Se(NMe₂)Cl, whereas with (Me₃Si)₂NH the salt [Ph₂Se?N?SePh₂]Cl is formed. The infrared spectra are presented and discussed.     

Triorganoantimon- und Triorganobismutderivate von 2-Pyridincarbonsäure und 2-Pyridylessigsäure Kristall- und Molekülstrukturen von (C6H5)3Sb(O2C-2-C5H4N)2 und (CH3)3Sb(O2CCH2-2-C5H4N)2

Triorganoantimony and Triorganobismuth Derivatives of 2-Pyridinecarboxylic Acid and 2-Pyridylacetic Acid. Crystal and Molecular Structures of (C₆H₅)₃Sb(O₂C-2-C₅H₄N)₂ and (CH₃)₃Sb(O₂CCH₂-2-C₅H₄N)₂ Triorganoantimony and triorganobismuth dicarboxylates R₃M(O₂C-2-C₅H₄N)₂ (M = Sb, R = CH₃, C₆H₅, 4-CH₃OC₆H₄; M = Bi, R = C₆H₅, 4-CH₃C₆H₄) and (CH₃)₃Sb(O₂CCH₂-2-C₅H₄N)₂ have been prepared from (CH₃)₃Sb(OH)₂, R₃SbO (R = C₆H₅, 4-CH₃OC₆H₄), or R₃BiCO₃ (R = C₆H₅, 4-CH₃C₆H₄) and the appropriate heterocyclic carboxylic acid. Vibrational spectroscopic data indicate a trigonal bipyramidal environment of M the O(? C)-atoms of the carboxylate ligands being in the apical and three C atoms (of R) in the equatorial positions; in addition coordinative interaction occurs in the 2-pyridinecarboxylates between M and O(?C) of one and N of the other carboxylate ligand and in (CH₃)₃)Sb(O₂CCH₂-2-C₅H₄N)₂ between Sb and O(?C) of both carboxylate ligands. (C₆H₅)₃Sb(O₂C-2-C₅H₄N)₂/(CH₃)₃Sb(O₂CCH₂-2-C₅H₄N)₂ crystallize monoclinic [space group P2₁/c/P2₁/n; a = 892.6(9)/1043.4(6), b = 1326.9(6)/3166.2(18), c = 2233.1(9)/1147.5(7) pm, β = 99.74(8)°/97.67(5)° Z = 4/8; d(calc.) = 1.522/1.553 × Mg m^?3; V_cell = 2606.7 × 10⁶/3757.0 × 10⁶pm³, structure determination from 3798/4965 independent reflexions (F ≥ 4.0 σ(F))/(I ≥ 1.96 σ(I), R(unweighted) = 0.024/0.036]. Sb is bonding to three C₆H₅/CH₃ groups in the equatorial plane [mean distances Sb? C: 212.2(3)/208.7(6) pm] and two carboxylate ligands via O in the apical positions [Sb? O distances: 218.5(2), 209.9(2)/212.1(3), 213.2(3) pm]. In (C₆H₅)₃Sb(O₂C-2-C₅H₄N)₂ there is a short Sb? O(?C) and a short Sb? N contact [Sb? O: 272.1(2), Sb? N: 260.2(2) pm] and distoritions of the equatorial angles [C? Sb? C: 99.2(1)°, 158.2(1)°, 102.0(1).] and of the axial angle [O? Sb? O: 169.9(1)°], and in (CH₃)₃Sb(O₂CCH₂-2-C₅H₄N)₂, which contains two different molecules in the asym-metric unit, there are two Sb? O(?C) contacts [Sb? O, mean: 302.2(4), and 310.7(4)pm, respectively] and distortions of the equatorial angles [C? Sb? C: 114.5(2)°, 132.4(3)° 113.1(2)°, and 123.9(3)° 115.5(2)°, 120.6(3)°, respectively] and of the axial angles [O? Sb? O: 174,9(1)°, 177.9(1)°, respectively].