Highly reduced organometallics: XII. The reaction of a carbonyltungstate anion with triphenyltin chloride resulting in a phenyltin bond cleavage. X-ray structural characterization of the novel salt: [Me4N][(Ph3Sn)2{(Ph2Sn)2O-i-Pr}W(CO)3]

The reaction of a highly reduced tricarbonyltungstate species with triphenyltin chloride results in an unprecedented phenyl-tin cleavage and the formation of an unusual substituted carbonyl anion. The X-ray structure of [Me₄N][(Ph₃Sn)₂-{(Ph₂Sn)₂O-i-Pr}W(CO)₃] shows the presence of seven coordinate tungsten bound to three terminal carbonyl groups, two triphenyltin units and a previously unknown isopropoxo-bis(diphenyltin) bidentate ligand. The seven ligating atoms are disposed in an approximate 4 : 3 piano stool arrangement about the central tungsten atom. Crystal data: Space group P2₁/c, a 22.580(10), b 14.162(4), c 23.070(10) Å, β 114.21(4)°, Z = 4, V 6728(1) ų, ?(calc) 1.626 g cm^?3.     

The crystal and molecular structure of triphenylphosphoniodithio-carboxylato-ss'-carbonylbis (trikphenylphosphine) iridium(I) tetrafluoroborate [Ir(S2CPPh3) (CO) (PPh3)2]BF4.

Crystal and molecular structures of the title compound have been determined from a three-dimensional X-ray analysis using diffractometer data. The crystals are monoclinic, space group P2₁/c, with Z = 4 in a unit cell of dimensions a = 10.5876(9), b = 31.518(10), c = 16.2164(5) Å, β = 92.521(1)°. The observed and calculated densities are 1.38 and 1.374 g cm^-1 respectively. The crystals decompose under X-rays, and three crystals were required to complete data collection. The structure was solved and refined by convetional methods to final residuals R and R_w of 0.087 and 0.107 respectively.The crystals contain monomeric cations, and BF₄ anions. The iridium atom is in a distorted trigonal bipyramidal environment consisting of the two sulphur atoms (one axial, one equatorial) of a bidentate triphenylphosphoniodi-thiocarboxylate ligand, two triphenylphosphine groups (equatorial) and the carbonyl ligand (axial). The non-equivalent Ir-s distances are 2.377 and 2.307(5) Å, the Ir-P distances are 2.334, 2.331(5) Å. Within the zwitterion, the C-S distances are 1.66 and 1.70(2) Å, while P-C is 1.78(2) Å. The condensation of PPh₃ and CS₂ to form the PH₃P⁺-CS₂ zwitterion is in contrast to that predicted previously.It is probable that the other complexes of iridium and rhodium prepared in a similar manner [2] should now be reformulated as containing Ph₃P⁺-CS₂^- ligands.     

Die molekül- und kristallstruktur von trimethylzinnazid Me3SnN3

The electrophilic cleavage reaction of (Me₃Sn)₂CN₂ with the Me₃SiN₃ in diluted ethereal solution affords well-formed crystals of Me₃SnN₂ in excellent yield; the azide was investigated by single crystal X-ray methods. Me₃SnN₃ crystallizes in the pseudohexagonal space group P2/b2/n2₁/n with Z = 4, d_c = 1.960 g cm^?3; a = 1172.5(6); b = 679.5(4); c = 875.5(5) pm; V = 697.55 ų.A total of 480 unique non-zero reflections was obtained at room temperature; refining the structure with anisotropic temperature factors for all non-hydrogen atoms and with isotropic temperatures factors for the hydrodgen atoms resulted in a conventional R-value of 0.024. Exactly planar Me₃Sn-groups are linked in zig-zag-chains by linear N₃-groups while the tin atoms adopt almost ideal symmetric trigonal bipyramidal coordination; the methyl groups of the Me₃Sn moieties are arranged in a staggered conformation along the c-axes.     

Darstellung und schwingungsspektren von trimethylzinndiorganothiophosphinaten Me3SnOSPR′R″ (R′R″ = Me2, MePh,Ph2). Die kristallstruktur von Me3SnOSPMe2

A series of trimethyltin diorganothiophosphinates Me₃SnOSPR′R″ (R′R″ = Me₂, MePh, Ph₂) was prepared from (Me₃Sn)₂O and R′R″PSCl in cyclohexane solution. A close study of the vibrational spectra is given; ³¹P NMR and mass spectra are also reported. The structural investigation of Me₃SnOSPMe₂ by means of X-ray diffraction (R 5.2%, 1697 observed independent reflexions) shows the compound to consists of chains, in which planar SnMe₃ units and tetrahedral OSPMe₂ groups are linked by the O- and S-atoms of the thiophosphinate.     

Kristall- und molekülstruktur von hexaphenyldistannylselenid (C6H5)3SnSeSn(C6H5)3

The crystal and molecular structure of hexaphenylditin selenide (C₆H₅)₃SnSeSn(G₆H₅)₃ was determined by X-ray diffraction data and was refined to R  0.055. The compound is monoclinic, space group P2₁, with a  9.950(4), b  18.650(7), c  18.066(6) Å, β  106.81(4)°, Z  4. The two molecules in the asymmetric unit differ slightly in their conformations, both having approximate C₂ symmetry. Bond lengths and angles are: SnSe 2.526 (2.521(3) ? 2.538(3)) Å; SnC 2.138 (2.107(16)?2.168(19)) Å; SnSeSn 103.4(1)°, 105.2(1)°. There are only slight angular distortions at the SnSeC₃ tetrahedra (SeSnC angles: 104.3(5)?114.8(4)°). The bond data indicate essentially single bonds around the Sn atoms.     

Matrix Isolation and IR spectroscopy of stannylenes (CH3)2Sn and (CD3)2Sn

Free stannylenes Me₂Sn and (CD₃)₂Sn, generated thermally from the cyclic hexamers or by microwave discharge from Me₂SnH₂, are isolated by Argon matrix technique. All IR bands could be attributed to the important molecular vibrations by normal coordinate analysis. As shown by ab initio SCF calculations, Me₂Sn has a singlet groud state, the angle CSnC is 95.3°, the CSn bond length is 2.203 Å.     

The crystal structure of triphenyltin isothiocyanate

The crystal structure of Ph₃SnNCS has been determined by single crystal X-ray diffraction. The crystals are monoclinic, P2₁, a = 19.02(3), b = 11.67(2), c = 15.49(2)Å;, β = 95.64(10)°, Z = 8. The molecules are arranged in infinite zig-zag S…SnNCS…Sn&.sbnd; chains similar to those in Me₃SnNCS, but with slightly longer SnN, shorter SnS bonds, and almost planar SnC₃ units. Principal mean bond lengths and angles are: SnN, 2.22(5); NC, 1.17(8); CS, 1.58(7); SSn, 2.92(1); SnC, 2.09(3); CC, 1.38(2)Å; SnNCm 161(4); CSSn, 97(3); SSnN, 175(3) and CSnC, 119.8(1.5)°.     

(Me2NH2)[(Ph3Sn)3(MoO4)2], ein Triorganozinnmolybdat mit Schichtstruktur

(Me₂NH₂)[(Ph₃Sn)₃(MoO₄)₂], a Triorganotin Molybdate with Layer Structure The reaction of [(Ph₃Sn)₂MoO₄] with (Me₂NH₂)Cl in an acetonitrile/water mixture leads to the formation of (Me₂NH₂)[(Ph₃Sn)₃(MoO₄)₂] ( 1 ). ( 1 ) crystallizes in the space group Pca2₁ with a = 1967.0(4), b = 1353.1(2) and c = 2176.6(5) pm. In the crystal structure of 1 Ph₃SnO₂ bipyramides and MoO₄ tetrahedra are linked by corner sharing to give a layer structure. Additionally the layers are connected by O···H···N hydrogen bridges between MoO₄ groups and [Me₂NH₂]⁺ ions to give a 3D network structure.     

The formation and crystal and molecular structures of (η5-pentamethylcyclopentadienyl)(η5-cyclopentadienyl)dichloro-titanium, -zirconium and -hafnium

A reaction between (η⁵-C₅Me₅)TiCl₃ and C₅H₅Tl in benzene solution has afforded (η⁵-C₅Me₅)(η⁵-C₅H₅)TiCl₂ (I) in quantitative yield. (η⁵-C₅Me₅)(η⁵-C₅H₅)HfCl₂ (III) has been prepared in 83% yield from a reaction between (η⁵-C₅Me₅)HfCl₃ and C₅H₅Na·DME in refluxing toluene solution. The crystal and molecular structures of (η⁵-C₅Me₅)(η⁵-C₅H₅TiCl₂ (I), (η⁵-C₅Me₅)(η⁵-C₅H₅)ZrCl₂ (II) and (η⁵-C₅Me₅)(η⁵-C₅H₅HfCl₂ (III) have been determined from X-ray data measured by counter methods. The three compounds are isostructural, crystallizing in the orthorhombic space group Pnma. The cell constants are: (I): a 9.873(1), b 12.989(3), c 11.376(4) Å and D_calc 1.45 g cm^?3 for Z = 4; (II): a 9.930(3), b 13.231(9), c 11.628(3) Å and D_calc 1.58 g cm^?3 for Z = 4; (III): a 9.938(1), b 13.156(2), c 11.582(2) Å and D_calc 1.97 g cm^?3 for Z = 4. In each case the metal atom resides on a crystallographic mirror plane which bisects both cyclopentadienyl rings and the ClMCl bond angle. The MCl bond lengths are 2.3518(9) for I, 2.4421(9) for II and 2.415(1) Å for III. The metal—cyclopentadienyl and metal—pentamethylcyclopentadienyl bond distances average 2.38(5) and 2.42(2) Å for I, 2.50(4) and 2.53(2) Å for II, and 2.48(4) and 2.50(1) Å for III respectively.     

Polysilane derivatives of the transition metals II. The crystal and molecular structure of [tris(trimethylsilyl)silyl]pentacarbonylmanganese, (Me3Si)3SiMn(CO)5

The crystal and molecular structures of [tris(trimethylsilyl)silyl]pentacarbonylmanganese, (Me₃Si)₃SiMn(CO)₅, have been determined from three-dimensional X-ray data obtained by counter methods. The compound crystallizes in space group P$\text{1}$ of the triclinic system, with two molecules in a unit cell of dimensions: a = 9.002(2), b = 9.655(2), c = 15.639(3) Å, α = 83.66(1), β = 105.65(1), γ = 114.61(1)°.The observed and calculated densities are 1.20 (±0.03) and 1.23 g-cm^?3 respectively. Full-matrix least-squares refinement of the structure has led to a final value of the conventional R factor of 0.059 for the 818 independent reflections having F² > 3σ(F²).The coordination geometry about the manganese atom is approximately octahedral and, about the silicon atom bonded to the manganese atom, tetrahedral.The relative orientations of carbonyl and trimethylsilyl groups, when viewed down the MnSi bond, appear consistent with minimization of energy due to nonbonded interactions.Two of the equatorial carbonyl groups are displaced out of the equatorial plane towards the silicon ligand by 6°. The SiMn bond is 2.564(6) Å long and has no multiple character.     

Crystal structure of cerium(III) diammonium polyphosphate (NH4)2Ce(PO3)5

Cerium(III) diammonium polyphosphate, (NH₄)₂Ce(PO₃)₅, is triclinic P1 with the following unit cell dimensions: a = 7.241(5) Å, b = 13.314(8) Å, c = 7.241(5)Å, α = 90.35(5)°, β′ = 107.50(5)°, γ = 90.28(5)°, and Z = 2, V = 665.7 ų, D_x = 2.85 g/cm³. The crystal structure of this new type of polyphosphate has been solved and refined from 4130 independent reflections to a final R value 0.029. The most interesting feature of this salt is the existence of two infinite crystallographically nonequivalent (PO₃)^?_∞ chains, one running parallel to the a axis, the other along the c axis, both with a period of five tetrahedra. This compound seems to be the first example of a long chain polyphosphate with crystallographic independent chains.     

The reversible adduct formation of group III trialkyls with relatively involatile phosphines; X-ray crystal structures of (Me3M)2·(Ph2PCH2)2 (M = Al,Ga, In) and (Me3Al)3·(Ph2PCH2CH2)2PPh

The following adducts of Group III trialkyls with phosphines have been prepared, either by direct reaction in hydrocarbon solution or by displacement of ether from the metal trialkyl etherate: Me₃M·PPh₃ (M = Ga, In); Me₃In·P(2-MeC₆H₄)₃; (R₃M)₂·(Ph₂PCH₂)₂ (R = Me, M = Al, Ga, In; R = Et, M = Ga, In; R = Buⁱ, M = Al); (Me₃M)₃·(Ph₂PCH₂CH₂)₂PPh (M = Al, Ga, In) and (Me₃M)₄·(Ph₂PCH₂CH₂PPhCH₂)₂ (M = Al, Ga, In). The compounds were analysed by ¹H and ³¹P NMR spectra of (Me₃M)₂·(Ph₂PCH₂)₂ (M = Ga, In) showed little change between 193 K and room temperature. Thermal dissociation of the adducts in vacuo gave the free metal trialkyl with no detectable contamination by the respective phosphine. Crystals of (Me₃M)₂·(Ph₂PCH₂)₂ (M = Al, Ga, In) are iso-structural and the molecules contain two distorted tetrahedral metals bridged by the (Ph₂PCH₂)₂; the MP distances are 2.544(4), 2.546(4) and 2.755(4) Å, respectively. The X-ray crystal structure of (Me₃Al)₃·(Ph₂PCH₂CH₂)₂PPh shows the molecule to contain distorted tetrahedral aluminium atoms bonded to each of the three phosphorus atoms, with AlP distances of 2.536(9) and 2.510(9) Å for the terminal and central moieties, respectively; the unit cell contains two such molecules plus one benzene molecule (the crystallizing solvent).     

Crystal and molecular structure of [{Rh(C5Me5)}3Cl5np3]PF6 · 0.5 C3H8O

The crystal and molecular structure of the monoligand trimetallic complex [{Rh(C₅Me₅)}₃Cl₅np₃]PF₆ · 0.5 C₃H₈O (np₃  tris(2-diphenylphosphinoethyl)-amine) have been established by a single-crystal X-ray diffraction study. The cation of the complex contains two Rh(C₅Me₅)Cl₂ units each bound through the metal to one phosphorus atom of the ligand and a Rh(C₅Me₅)Cl group in which the rhodium is bound to the third phosphorus atom and to the nitrogen of the tetradentate ligand.The crystals are triclinic, space group P$\text{1}$, with cell dimensions a 28.598(8), b 13.757(4), c 10.748(3) Å, α 90.69(4), β 96.67(4), γ 99.71(4)°, D_c 1.38 g cm^?3 for Z  2. The structure was solved by three dimensional Patterson and Fourier syntheses and refined by least-squares techniques to a final conventional R value of 0.098.     

New hydrogen-bonded dimeric and polymeric gold(I) complexes of the heterodifunctional ligand Ph2PNHP(O)Ph2

The preparation of several new gold(I) complexes by chloride metathesis of [AuCl(HL)] [HL=Ph₂PNHP(O)Ph₂] with either HL or K[Ph₂P(E)NP(E)Ph₂] (E=S or Se) is described. All compounds were characterised by a combination of ³¹P{¹H}, ¹H and IR spectroscopy, microanalysis and X-ray crystallography. X-ray structural studies reveal that [Au(HL)₂]Cl [monoclinic, space group P2₁/c, a=9.0726(3) Å, b=21.0847(6) Å, c=12.0131(3) Å, β=105.1090(10)°, V=2219 ų, Z=2, final R=3.97] forms a one dimensional polymeric structure in which alternating [Au(HL)₂]⁺ and Cl⁻ ions are linked through intermolecular N–H⋯Cl hydrogen-bonding. In contrast the three-co-ordinate compound [Au{Ph₂P(Se)NP(Se)Ph₂-Se,Se′}(HL)] [monoclinic, space group P2₁/a, a=21.6752(5) Å, b=9.1200(10) Å, c=24.0742(7) Å, β=106.080(2)°, V=4573 ų, Z=4, final R=8.94] forms hydrogen-bonded dimer pairs analogous to that previously observed in non-complexed HL. The X-ray crystal structure of the gold(I) precursor [AuCl(HL)] has also been determined: monoclinic, space group P2₁/c, a=10.217(8) Å, b=23.256(5) Å, c=20.086(5) Å, β=101.15(4)°, V=4683 ų, Z=8, final R=5.2. The X-ray crystal structure reveals intermolecular N–H⋯OP hydrogen-bonding between adjacent [AuCl(HL)] molecules forming infinite chains.     

The crystal and molecular structure of Rh2(CH3CO2)4[HCON(CH3)]2—effect of ligands on metalmetal bonding

The structure of Rh₂(CH₃CO₂)₄(DMF)₂ {DMF = HCON(CH₃)₂} has been determined by single crystal X-ray methods. The compound crystallizes with eight formula units in a cell of dimensions: a = 29.438(7) Å, b = 7.978(2) Å, c = 20.279(5) Å, β = 113.20(4)°, V = 4377.5 ų, space group C2/c. The structure has been refined by full-matrix least-squares method to a final R = 0.030 for the 4156 observed data. Two Rh(II) atoms are linked by four acetate groups forming a dimeric unit, where the RhRh distance is 2.383(1) Å. The coordination sphere about each Rh atom is completed by a DMF molecule; the average RhO(DMF) distance is 2.296(3) Å.     

Skew-trapezoidal bipyramidal diorganotin(IV) bischelates. Crystal structure of dimethylbis(2-pyridinethiolato-N-oxide)tin(IV)

Dimethylbis(2-pyridinethiolato-N-oxide)tin(IV), Me₂Sn(2-SPyO)₂, crystallizes in space group P2₁/c with a 9.877(3), b 11.980(4), c 13.577(3) Å, β 109.1(2)° and Z = 4. The structure was refined to R_F = 0.036 for 2263 Mo-K_α observed reflections. The coordination geometry at tin is a skew-trapezoidal bipyramid, with the oxygen [SnO 2.356(3), 2.410(4) Å] and sulfur [SnS 2.536(1), 2.566(1) Å] atoms of the chelating groups occupying the trapezoidal plane and the methyl groups [SnC 2.106(6), 2.128(7) Å] occupying the apical positions. The methyl-tin-methyl skeleton is bent [CSnC 138.9(2)°]. The SSnS angle is 77.8(1)°, but the OSnO angle is opened to 136.7(1)° to accommodate the intruding methyl groups. The carbontincarbon angles predicted from quadrupole splitting (^119mSn Mössbauer) and one-bond ¹¹⁹Sn¹³C coupling constant (solution ¹³C NMR) data agree closely with the experimental value.     

Structural studies of complexes containing the coordinated methyldisulphido ligand: The crystal structure of [Os (η2-S2CH3) (CO)2 (P (C6H5)3)2] ClO4·12 C6H6.

Crystal and molecular structures of the title compound have been determined from a three-dimentional X-ray analysis usinq diffractometer data. The crystals are triclinic, space group P$\text{1}$, with Z = 2 in a unit cell of dimensions a = 14.23(1), b = 17.30(1), c = 10.44(1) Å, α = 102.1(2), β = 102.7(2), γ = 105.5(2)°. Full matrix least squares refinement has given a final R-factor of 0.060 for 4628 reflections for which I > 3σ(I).The crystal structure consist of discrete cations and anions, together with benzene molecules of crystallisation which are situated about the crystallographic centres of symmetry and serve a purely space-filling role. In the cation coordination about the osmium atom is that of a distorted octahedron, comprising the two triphenylphosphine groups (mutually trans), the two carbonyl groups (mutually cis) and the dihapto S₂Me group. The Os-P distances of 2.420 and 2.419(3) Å are normal. The S₂Me group is nearly symmetrically coordinated with Os-S(l) 2.426(4)Å and Os-S(3) 2.442(4) Å. Other bonds and angles in this ligand are S(1)-S(2) 2.022(7) Å, S(1)-CH₂ 1.81(2) Å, and S(2)-S(1)-CH₃ 105.4(6)°. The observed geometry is similar to that in [Ir(S₂) (Ph₂PCH₂CH₂PPh₂)₂Cl.Ch₃CN.     

Crystal and molecular structure of tricyclopentadienyltetrahydrofuranuranium(III), (η5-C5H5)3U·OC4H8

Tricyclopentadienyltetrahydrofuranuranium(III), (η⁵-C₅H₅)₃U·OC₄H₈, crystallizes in the centrosymmetric monoclinic space group P2₁/n with a 8.248(3), b 24.322(17), c 8.357(4) Å, β 101.29(5)°, V 1644.0 ų and ρ(calc) 2.04 g cm^?1 for Z = 4 and mol.wt. 595.0. Diffraction data (Mo-K_α, 2θ(max) 45°) were collected on an Enraf-Nonius CAD4 diffractometer and the structure was refined to R_w(F) 4.7% for those 1530 reflections having I > 2σ(I). The molecule consists of a distorted tetrahedral arrangement of THF and (η⁵-C₅H₅) ligands with CpUCp angles in the range 110.4–122.4° and CpUO angles between 90.2 and 106.0°. Individual uranium-carbon distances range from 2.76(2) to 2.82(2) Å and average 2.79[1] Å. The uranium-oxygen distance of 2.551(10) Å suggests a 10-coordinate U³⁺ radius of 1.20 Å in this class of compounds.     

Synthesis and structure of the heterotrinuclear chromium-palladium clusters (RC5H4CrCl)2-(μ3S)(μ-SCMe3)2Pd(PPh3) with ferromagnetic exchange interactions over the CrSCr system

Reactions of (RC₅H₄)₂Cr₂(SCMe₃)₂S(I, R = H; II, R = Me) with (PPh₃)₂PdCl₂ in benzene at 20°C gives trinuclear complexes (RC₅H₄)₂Cr₂Cl₂(μ₃-S)(μ-SCMe₃)₂Pd(PPh₃)(III, R = H; IV, R = Me). The structure of IV as a monobenzene solvate is established by an X-ray analysis (black-green triclinic crystals space group P$\text{1}$ with a = 11.403(4), b = 14.933(5), c = 14.131(5) Å, α = 99.13(3), β = 112.72(3), γ = 95.65(3)°, V = 2201.6 Å, Z = 2; IV·C₆H₆). The structure was solved by direct methods and refined in an anisotropic approximation to R = 0.046, R_w = 0.058 for 7643 reflections with I ? 2σ(I). In the molecule of IV metal atoms are separated by non-bonding distances (Cr … Cr 4.079(I), Cr … Pd 3.230(I) and 3.380(I) Å) but linked by the bridging tridentate sulphur atom (CrS 2.339(2) and 2.329(2), PdS 2.327(2) Å), and two SCMe₃ groups between Pd and Cr (CrS 2.396(2) and 2.403(2), PdS 2.350(2) and 2.381(2) Å, Cr?Pd 85.14(6) and 89.92(6)°). The Cl atoms are transferred from Pd to Cr atoms (CrCl 2.308(2) Å) and being terminally coordinated are in trans-positions to each other (as well as η-CH₃C₅H₄ rings) with respect to the Cr₂Pd plane. Cr atoms in III and IV exhibit ferromagnetic exchange interactions over the Cr?Cr system (+2J = 28 and 11 cm^?1, respectively).     

Die Reaktionen von M[BF4] (M = Li,K) und (C2H5)2O·BF3 mit (CH3)3SiCN. Bildung von M[BFx>(CN)4—x] (M = Li,K; x = 1, 2) und (CH3)3SiNCBFx(CN)3—x, (x = 0, 1)

The Reactions of M[BF₄] (M = Li, K) and (C₂H₅)₂O·BF₃ with (CH₃)₃SiCN. Formation of M[BF_x(CN)_4—x] (M = Li, K; x = 1, 2) and (CH₃)₃SiNCBF_x(CN)_3—x, (x = 0, 1) The reaction of M[BF₄] (M = Li, K) with (CH₃)₃SiCN leads selectively, depending on the reaction time and temperature, to the mixed cyanofluoroborates M[BF_x(CN)_4—x] (x = 1, 2; M = Li, K). By using (C₂H₅)₂O·BF₃ the synthesis yields the compounds (CH₃)₃SiNCBF_x(CN)_3—x x = 0, 1. The products are characterized by vibrational and NMR‐spectroscopy, as well as by X‐ray diffraction of single‐crystals: Li[BF₂(CN)₂]·2Me₃SiCN Cmc2₁, a = 24.0851(5), b = 12.8829(3), c = 18.9139(5) Å V = 5868.7(2) ų, Z = 12, R₁ = 4.7%; K[BF₂(CN)₂] P4₁2₁2, a = 13.1596(3), c = 38.4183(8) Å, V = 6653.1(3) ų, Z = 48, R₁ = 2.5%; K[BF(CN)₃] P1¯, a = 6.519(1), b = 7.319(1), c = 7.633(2) Å, α = 68.02(3), β = 74.70(3), γ = 89.09(3)°, V = 324.3(1) ų, Z = 2, R₁ = 3.6%; Me₃SiNCBF(CN)₂ Pbca, a = 9.1838(6), b = 13.3094(8), c = 16.840(1) Å, V = 2058.4(2) ų, Z = 8, R₁ = 4.4%