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While exploring the chemistry of tellurium-containing dichalcogenidoimido­diphosphinate ligands, the first all-tellurium member of a series of related square-planar EII(E')4 complexes (E and E' are group 16 elements), namely bis­(P,P,P',P'-tetra­phenyl­ditelluridoimidodiphosphinato-[kappa]2Te,Te')tellurium(II) (systematic name: 2,2,4,4,8,8,10,10-octa­phenyl-1[lambda]3,5,6[lambda]4,7[lambda]3,11-pentatellura-3,9-di­aza-2[lambda]5,4[lambda]5,8[lambda]5,10[lambda]5-tetra­phospha­spiro­[5.5]undeca-1,3,7,9-tetra­ene), C48H40N2P4Te5, was obtained unexpectedly. The formally TeII centre is situated on a crystallographic inversion centre and is Te,Te'-chelated to two anionic [(TePPh2)2N]- ligands in an anti conformation. The central TeII(Te)4 unit is approximately square planar [Te-Te-Te = 93.51 (3) and 86.49 (3)°], with Te-Te bond lengths of 2.9806 (6) and 2.9978 (9) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229615007949/yp3092sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229615007949/yp3092Isup2.hkl
Contains datablock I

cml

Chemical Markup Language (CML) file https://doi.org/10.1107/S2053229615007949/yp3092Isup3.cml
Supplementary material

CCDC reference: 1060938

Introduction top

Dichalcogenidoimidodiphosphinates, [(EPR2)2N] (E = O, S, Se, Te; R = alkyl, aryl), are versatile ligands that can coordinate to elements from the main group (Silvestru & Drake, 2001), d-block (Ly and Woollins, 1998) and f-block (Glover et al., 2007). These species can be viewed as flexible inorganic analogues to planar β-diketonate ligands, and many derivatives are known owing to the varying identities possible for the chalcogen and organic substituents on phospho­rus. In keeping with this versatility, these ligands have demonstrated a wealth of different coordination modes and solid-state structures in combination with metals.

We have been exploring the chemistry of the rarer tellurium-containing ligands since reporting a route to the synthesis of their sodium salts (Briand et al., 2002). In addition to studying their coordination chemistry (Chivers et al., 2010), the one-electron chemical oxidation of these anions with iodine was pursued in the context of forming ditelluride dimers. The iso­propyl-substituted ligand forms a symmetric dimer, (I), with an unusually long Te—Te distance (Chivers et al., 2005), while the tert-butyl analogue forms an asymmetric dimer, (II) (Ritch et al., 2007), resembling a contact ion pair between a cation and anion (Fig. 1). In this work, an unexpected product, obtained by the oxidation of the phenyl-substituted ligand [(TePPh2)2N]-, is reported as bis­(P,P,P',P'-tetra­phenyl­ditelluridoimidodiphosphinato-κ2Te,Te')tellurium(II), (III).

Experimental top

Synthesis and crystallization top

To a solution of Na(tmeda)[(TePPh2)2N] (tmeda is tetra­methyl­ethylenedi­amine; 285 mg, 0.366 mmol) in tetra­hydro­furan (THF) at 195 K was added a solution of one-half molar equivalent of I2 (45 mg, 0.177 mmol) in THF at 195 K. The resulting mixture was stirred cold for 30 min and then warmed to room temperature for an additional 30 min. The volatiles were removed under vacuum and the residual material was then extracted with toluene and filtered through a 0.45 µm pore size PTFE filter disk. Removal of the volatiles afforded a red solid (60 mg), which was shown to be a complicated mixture of phospho­rus-containing compounds (ten resonances in the 31P NMR spectrum). A few X-ray quality red block-like crystals of Te[(TePPh2)2N]2, (III), were obtained from a THF solution layered with n-hexane and stored at 278 K. All solvents were dried (THF and toluene with sodium/benzo­phenone, andn-hexane with sodium), distilled and stored over 4 Å molecular sieves prior to use, and all manipulations were conducted under argon using a glove-box or Schlenk line.

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1. Three of the four phenyl rings in the asymmetric unit exhibit positional disorder and were modelled as isotropic mixtures over two positions. The occupancy factors for the disordered atoms were determined by free variable refinement, and yielded values of ca 0.5. FLAT restraints were applied to four half-occupancy isotropic rings. [Please avoid program specific commands and describe the restraint instead] H atoms were placed in calculated positions, with C—H = 0.95 Å and Uiso(H) = 1.2Ueq(C), and treated with a riding-model approximation.

Results and discussion top

The complex mixture obtained in the oxidation of the phenyl-substituted ditelluridoimidodiphosphinate anion is in contrast to the alkyl-substituted derivatives (R = iPr, t-Bu), for which the corresponding reactions with iodine were quite clean (Chivers et al., 2005; Ritch et al., 2007). The red crystals obtained from this mixture possess a molecular spiro­cyclic square-planar TeII(Te)4 motif (Fig. 2), of which only a few examples are known.

Some extended structures exhibit square-planar Te5 units, such as the anions in the previously-reported salt [NMe4]2[As2Te5], which contains alternating Te56- and As24+ groups in one-dimensional chains (Warren et al., 1994). A spiro­cyclic Te82- anion is seen in the structure of [K(18-crown-5)2]2[Te8] (Schreiner et al., 1993). More recently, the Te5 unit was oberved in [Na(tmeda)]2[{(t-Bu)N(Te)P[µ-N(t-Bu)]2P(Te)N(t-Bu)}24-Te], (IV) (tmeda is tetra­methyl­ethylenedi­amine) (Nordheider et al., 2015), which can be described as a Te2+ cation bound by two Te,Te'-chelating dianionic ligands. In this structure, the Te—Te distances range from 3.014 (2) to 3.027 (2) Å an, while the Te5 unit is planar, the cis-Te—Te—Te bond angles range from 74.47 (4) to 105.61 (5)°.

The title compound, (III), features slightly shorter bond lengths, with Te1—Te3 and Te2—Te3 distances of 2.9806 (6) and 2.9978 (9) Å, respectively, which are still significantly longer than the distances observed in organic ditellurides [e.g. 2.712 (2) Å in Ph2Te2; Llabres et al., 1972]. The geometry is also much closer to ideal square planar; the two unique cis-Te—Te—Te bond angles are 93.51 (3) and 86.49 (3)°. Compared to the dianionic ligands in (IV), which feature rigid P2N2 rings, the [(TePPh2)2N]- ligands in (III) are considerably more flexible, as seen from the Te—P—N—P torsion angles [-9.3 (5) and 67.9 (4)°]. This flexibility may be the reason the geometry of the Te(Te)4 core is closer to ideal square planar than that in (IV).

The bonding parameters of the [(TePPh2)2N]- ligands are indicative of delocalization of π-electron density within the TePNPTe fragment. The P—Te distances of 2.4278 (16) and 2.4331 (15) Å are equal within experimental error, and are significantly longer than a formal double PTe bond, e.g. the distance of 2.3798 (8) Å in the monotelluridoimidodiphosphinate, TePiPr2NP(H)iPr2 (Chivers et al., 2005). The P—N inter­atomic distances of 1.593 (5) and 1.594 (5) Å are shorter the formally single P—N bonds observed in the di­seleno­imidodiphosphinate (SePPh2)2NH [1.678 (4) and 1.686 (3) Å; Bhattacharyya et al., 1995], and the P—N—P bond angle is 134.1 (3)°. Together, these data suggest partial multiple bond character throughout the ligand backbone, which is consistent with other structures containing [(EPR2)2N]- anions (E = O, S, Se, Te; R = alkyl, aryl).

Square-planar Te(E)4 (E = S, Se) complexes involving dichalcogenidoimidodiphosphinates have been observed previously [e.g. TeS4 (Bjørnvåg et al., 1982; Birdsall et al., 2000; Necas et al., 2001), TeSe4 (Novosad et al., 1998; Birdsall et al., 2000), TeS2Se2 (Sekar & Ibers, 2003)], however, compound (III) is the first example of a TeII(Te)4 imidodiphosphinate complex. Similar to the previously reported complexes, the two ligands in (III) are in an anti conformation with respect to each other.

Computing details top

Data collection: COLLECT (Nonius, 2001); cell refinement: DENZO (Nonius, 2001); data reduction: DENZO (Nonius, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2008); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Figures top
[Figure 1] Fig. 1. Displacement ellipsoid plot (50% probability level) of the structure of (III). H atoms have been omitted for clarity and spheres indicate isotropic C atoms from one orientation of the disordered phenyl rings. Symmetry-equivalent atoms are related by an inversion centre at Te3. [Symmetry code: (A) -x+2, -y+1, -z.] [Please provide a fully labelled plot; the symmetry-generated half need not be labelled any further]
2,2,4,4,8,8,10,10-Octaphenyl-1λ3,5,6λ4,7λ3,11-pentatellura-3,9-diaza-2λ5,4λ5,8λ5,10λ5-tetraphosphaspiro[5.5]undeca-1,3,7,9-tetraene top
Crystal data top
C48H40N2P4Te5F(000) = 1324
Mr = 1406.70Dx = 1.945 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 11.021 (2) ÅCell parameters from 41094 reflections
b = 14.950 (3) Åθ = 2.7–25.0°
c = 15.893 (3) ŵ = 3.17 mm1
β = 113.47 (3)°T = 173 K
V = 2402.2 (10) Å3Block, red
Z = 20.02 × 0.02 × 0.02 mm
Data collection top
Nonius KappaCCD
diffractometer
3159 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
ϕ and ω scansθmax = 25.0°, θmin = 2.7°
Absorption correction: integration
(SCALEPACK; Otwinowski & Minor, 1997)
h = 1313
Tmin = 0.939, Tmax = 0.939k = 1717
8246 measured reflectionsl = 1818
4216 independent reflections
Refinement top
Refinement on F212 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.034H-atom parameters constrained
wR(F2) = 0.083 w = 1/[σ2(Fo2) + (0.0334P)2 + 3.8459P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.002
4216 reflectionsΔρmax = 0.60 e Å3
253 parametersΔρmin = 0.71 e Å3
Crystal data top
C48H40N2P4Te5V = 2402.2 (10) Å3
Mr = 1406.70Z = 2
Monoclinic, P21/cMo Kα radiation
a = 11.021 (2) ŵ = 3.17 mm1
b = 14.950 (3) ÅT = 173 K
c = 15.893 (3) Å0.02 × 0.02 × 0.02 mm
β = 113.47 (3)°
Data collection top
Nonius KappaCCD
diffractometer
4216 independent reflections
Absorption correction: integration
(SCALEPACK; Otwinowski & Minor, 1997)
3159 reflections with I > 2σ(I)
Tmin = 0.939, Tmax = 0.939Rint = 0.033
8246 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03412 restraints
wR(F2) = 0.083H-atom parameters constrained
S = 1.08Δρmax = 0.60 e Å3
4216 reflectionsΔρmin = 0.71 e Å3
253 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Te11.04321 (4)0.36828 (3)0.15000 (3)0.04004 (13)
Te21.26616 (4)0.58511 (3)0.09597 (3)0.04165 (13)
Te31.00000.50000.00000.03290 (14)
P11.05091 (14)0.48895 (9)0.25423 (10)0.0310 (3)
P21.29607 (13)0.56634 (9)0.25510 (9)0.0302 (3)
N11.1666 (4)0.5605 (3)0.2763 (3)0.0344 (11)
C11.0619 (5)0.4377 (4)0.3609 (4)0.0324 (13)
C21.1378 (6)0.4791 (4)0.4437 (4)0.0431 (15)
H21.18270.53340.44390.052*
C31.1476 (7)0.4415 (5)0.5252 (5)0.0582 (19)
H31.20200.46910.58140.070*
C41.0799 (8)0.3644 (5)0.5263 (5)0.062 (2)
H41.08590.33970.58290.074*
C51.0031 (8)0.3234 (4)0.4444 (5)0.060 (2)
H50.95660.26990.44470.072*
C60.9936 (7)0.3599 (4)0.3621 (5)0.0515 (17)
H60.94010.33160.30600.062*
C70.898 (2)0.5566 (13)0.2135 (9)0.028 (7)*0.507 (13)
C80.9012 (13)0.6397 (8)0.1819 (8)0.036 (3)*0.507 (13)
H80.98150.66340.18230.044*0.507 (13)
C90.7878 (12)0.6901 (9)0.1490 (8)0.042 (3)*0.507 (13)
H90.79000.74860.12630.050*0.507 (13)
C100.6738 (18)0.6578 (12)0.1483 (9)0.050 (5)*0.507 (13)
H100.59600.69340.12590.059*0.507 (13)
C110.6700 (13)0.5693 (9)0.1816 (9)0.047 (4)*0.507 (13)
H110.58980.54570.18130.056*0.507 (13)
C120.7852 (11)0.5183 (8)0.2144 (8)0.039 (3)*0.507 (13)
H120.78580.45920.23660.046*0.507 (13)
C7A0.897 (2)0.5446 (15)0.2063 (10)0.026 (7)*0.493 (13)
C8A0.8894 (14)0.6383 (9)0.2152 (9)0.044 (4)*0.493 (13)
H8A0.96840.67180.24470.052*0.493 (13)
C9A0.7678 (15)0.6824 (10)0.1812 (9)0.050 (4)*0.493 (13)
H9A0.76430.74540.18720.060*0.493 (13)
C10A0.6512 (16)0.6335 (11)0.1383 (9)0.037 (4)*0.493 (13)
H10A0.56810.66310.11650.044*0.493 (13)
C11A0.6563 (12)0.5465 (8)0.1282 (8)0.040 (3)*0.493 (13)
H11A0.57700.51380.09720.048*0.493 (13)
C12A0.7759 (11)0.5025 (8)0.1621 (8)0.035 (3)*0.493 (13)
H12A0.77540.43940.15490.042*0.493 (13)
C131.3903 (19)0.6627 (12)0.3096 (12)0.025 (6)*0.47 (4)
C141.5141 (16)0.6797 (11)0.3150 (16)0.043 (5)*0.47 (4)
H141.55230.64010.28570.051*0.47 (4)
C151.5863 (16)0.7525 (10)0.3617 (15)0.042 (5)*0.47 (4)
H151.67230.76260.36320.051*0.47 (4)
C161.5365 (19)0.8087 (11)0.4047 (10)0.033 (5)*0.47 (4)
H161.58920.85710.43860.040*0.47 (4)
C171.412 (2)0.7985 (10)0.4014 (10)0.035 (4)*0.47 (4)
H171.37630.83930.43140.042*0.47 (4)
C181.336 (2)0.7235 (16)0.3506 (15)0.042 (7)*0.47 (4)
H181.24770.71550.34520.050*0.47 (4)
C13A1.3736 (17)0.6690 (12)0.3191 (12)0.027 (5)*0.53 (4)
C14A1.5115 (14)0.6797 (10)0.3414 (13)0.038 (4)*0.53 (4)
H14A1.55950.63630.32340.046*0.53 (4)
C15A1.5741 (15)0.7563 (10)0.3906 (13)0.042 (4)*0.53 (4)
H15A1.66600.76540.40720.051*0.53 (4)
C16A1.499 (2)0.8196 (10)0.4153 (10)0.037 (4)*0.53 (4)
H16A1.53960.87230.44750.045*0.53 (4)
C17A1.365 (2)0.8045 (9)0.3923 (9)0.038 (4)*0.53 (4)
H17A1.31350.84700.40850.046*0.53 (4)
C18A1.308 (2)0.7299 (11)0.3472 (12)0.031 (5)*0.53 (4)
H18A1.21730.71940.33440.037*0.53 (4)
C191.4013 (15)0.4821 (11)0.3088 (12)0.028 (6)*0.478 (19)
C201.4711 (12)0.4284 (8)0.2699 (8)0.026 (3)*0.478 (19)
H201.45570.43800.20730.031*0.478 (19)
C211.5617 (14)0.3617 (9)0.3181 (9)0.037 (4)*0.478 (19)
H211.60770.32770.28970.044*0.478 (19)
C221.5817 (15)0.3474 (10)0.4103 (11)0.037 (5)*0.478 (19)
H221.63960.30090.44400.044*0.478 (19)
C231.5227 (14)0.3964 (11)0.4504 (13)0.054 (4)*0.478 (19)
H231.54220.38700.51360.065*0.478 (19)
C241.4321 (12)0.4618 (10)0.4031 (10)0.038 (4)*0.478 (19)
H241.38870.49430.43440.046*0.478 (19)
C19A1.4201 (15)0.4712 (9)0.3069 (10)0.026 (5)*0.522 (19)
C20A1.5171 (14)0.4543 (9)0.2756 (8)0.042 (3)*0.522 (19)
H20A1.52040.48530.22440.051*0.522 (19)
C21A1.6107 (15)0.3895 (9)0.3224 (8)0.046 (4)*0.522 (19)
H21A1.67860.37540.30200.055*0.522 (19)
C22A1.6070 (15)0.3472 (9)0.3946 (9)0.036 (4)*0.522 (19)
H22A1.67430.30520.42630.044*0.522 (19)
C23A1.5020 (14)0.3639 (10)0.4264 (10)0.046 (4)*0.522 (19)
H23A1.49730.33160.47650.055*0.522 (19)
C24A1.4088 (13)0.4290 (9)0.3805 (9)0.041 (3)*0.522 (19)
H24A1.33960.44390.39940.049*0.522 (19)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Te10.0506 (3)0.0344 (2)0.0348 (2)0.00087 (18)0.01672 (19)0.00028 (17)
Te20.0320 (2)0.0580 (3)0.0303 (2)0.00880 (18)0.00750 (17)0.00862 (18)
Te30.0310 (3)0.0380 (3)0.0280 (3)0.0006 (2)0.0099 (2)0.0024 (2)
P10.0284 (8)0.0322 (8)0.0328 (8)0.0008 (6)0.0126 (6)0.0018 (6)
P20.0248 (7)0.0330 (8)0.0279 (7)0.0034 (6)0.0053 (6)0.0040 (6)
N10.030 (2)0.036 (3)0.037 (3)0.005 (2)0.013 (2)0.001 (2)
C10.028 (3)0.035 (3)0.033 (3)0.004 (2)0.012 (2)0.007 (3)
C20.038 (3)0.058 (4)0.034 (3)0.004 (3)0.015 (3)0.004 (3)
C30.055 (4)0.082 (5)0.036 (4)0.013 (4)0.017 (3)0.011 (4)
C40.077 (5)0.069 (5)0.052 (5)0.027 (4)0.038 (4)0.025 (4)
C50.094 (6)0.037 (4)0.070 (5)0.005 (4)0.054 (5)0.018 (4)
C60.065 (4)0.038 (4)0.054 (4)0.005 (3)0.026 (4)0.004 (3)
Geometric parameters (Å, º) top
Te1—Te32.9806 (6)C11A—C12A1.376 (16)
Te1—P12.4278 (16)C12A—H12A0.9500
Te2—Te32.9978 (9)C13—C141.36 (2)
Te2—P22.4331 (15)C13—C181.39 (3)
Te3—Te1i2.9806 (6)C14—H140.9500
Te3—Te2i2.9979 (9)C14—C151.38 (2)
P1—N11.593 (5)C15—H150.9500
P1—C11.820 (6)C15—C161.33 (2)
P1—C71.85 (2)C16—H160.9500
P1—C7A1.77 (2)C16—C171.36 (2)
P2—N11.594 (5)C17—H170.9500
P2—C131.786 (18)C17—C181.44 (3)
P2—C13A1.851 (17)C18—H180.9500
P2—C191.695 (19)C13A—C14A1.43 (2)
P2—C19A1.917 (17)C13A—C18A1.34 (3)
C1—C21.392 (8)C14A—H14A0.9500
C1—C61.390 (8)C14A—C15A1.40 (2)
C2—H20.9500C15A—H15A0.9500
C2—C31.376 (9)C15A—C16A1.41 (2)
C3—H30.9500C16A—H16A0.9500
C3—C41.377 (10)C16A—C17A1.39 (2)
C4—H40.9500C17A—H17A0.9500
C4—C51.382 (10)C17A—C18A1.34 (2)
C5—H50.9500C18A—H18A0.9500
C5—C61.383 (9)C19—C201.41 (2)
C6—H60.9500C19—C241.43 (2)
C7—C81.35 (2)C20—H200.9500
C7—C121.38 (2)C20—C211.402 (16)
C8—H80.9500C21—H210.9500
C8—C91.372 (17)C21—C221.41 (2)
C9—H90.9500C22—H220.9500
C9—C101.34 (2)C22—C231.30 (2)
C10—H100.9500C23—H230.9500
C10—C111.43 (2)C23—C241.39 (2)
C11—H110.9500C24—H240.9500
C11—C121.393 (17)C19A—C20A1.37 (2)
C12—H120.9500C19A—C24A1.38 (2)
C7A—C8A1.41 (3)C20A—H20A0.9500
C7A—C12A1.39 (2)C20A—C21A1.394 (17)
C8A—H8A0.9500C21A—H21A0.9500
C8A—C9A1.40 (2)C21A—C22A1.33 (2)
C9A—H9A0.9500C22A—H22A0.9500
C9A—C10A1.40 (2)C22A—C23A1.46 (2)
C10A—H10A0.9500C23A—H23A0.9500
C10A—C11A1.31 (2)C23A—C24A1.392 (18)
C11A—H11A0.9500C24A—H24A0.9500
P1—Te1—Te390.34 (4)C10A—C11A—C12A120.4 (13)
P2—Te2—Te3100.37 (4)C12A—C11A—H11A119.8
Te1—Te3—Te1i180.0C7A—C12A—H12A118.0
Te1—Te3—Te293.51 (3)C11A—C12A—C7A124.0 (13)
Te1—Te3—Te2i86.49 (3)C11A—C12A—H12A118.0
Te1i—Te3—Te286.49 (3)C14—C13—P2123.9 (14)
Te1i—Te3—Te2i93.51 (3)C14—C13—C18117.3 (17)
Te2—Te3—Te2i180.0C18—C13—P2118.7 (15)
N1—P1—Te1117.19 (18)C13—C14—H14118.9
N1—P1—C1109.1 (3)C13—C14—C15122.3 (17)
N1—P1—C7104.3 (6)C15—C14—H14118.9
N1—P1—C7A109.0 (7)C14—C15—H15119.8
C1—P1—Te1107.11 (19)C16—C15—C14120.4 (15)
C1—P1—C7105.7 (5)C16—C15—H15119.8
C7—P1—Te1112.9 (4)C15—C16—H16119.2
C7A—P1—Te1106.8 (6)C15—C16—C17121.7 (15)
C7A—P1—C1107.3 (5)C17—C16—H16119.2
N1—P2—Te2117.66 (18)C16—C17—H17121.3
N1—P2—C13109.8 (7)C16—C17—C18117.4 (16)
N1—P2—C13A100.7 (7)C18—C17—H17121.3
N1—P2—C19110.1 (6)C13—C18—C17120.8 (18)
N1—P2—C19A114.4 (5)C13—C18—H18119.6
C13—P2—Te2102.9 (6)C17—C18—H18119.6
C13A—P2—Te2108.5 (5)C14A—C13A—P2116.3 (13)
C13A—P2—C19A106.6 (6)C18A—C13A—P2123.5 (13)
C19—P2—Te2113.1 (7)C18A—C13A—C14A120.2 (17)
C19—P2—C13101.9 (7)C13A—C14A—H14A121.0
C19A—P2—Te2108.1 (5)C15A—C14A—C13A118.0 (14)
P1—N1—P2134.1 (3)C15A—C14A—H14A121.0
C2—C1—P1119.0 (4)C14A—C15A—H15A120.4
C6—C1—P1122.0 (5)C14A—C15A—C16A119.3 (13)
C6—C1—C2118.9 (5)C16A—C15A—H15A120.4
C1—C2—H2120.0C15A—C16A—H16A120.1
C3—C2—C1120.0 (6)C17A—C16A—C15A119.9 (13)
C3—C2—H2120.0C17A—C16A—H16A120.1
C2—C3—H3119.5C16A—C17A—H17A120.2
C2—C3—C4120.9 (7)C18A—C17A—C16A119.6 (15)
C4—C3—H3119.5C18A—C17A—H17A120.2
C3—C4—H4120.3C13A—C18A—H18A118.5
C3—C4—C5119.5 (6)C17A—C18A—C13A123.0 (17)
C5—C4—H4120.3C17A—C18A—H18A118.5
C4—C5—H5119.9C20—C19—P2125.7 (13)
C4—C5—C6120.1 (7)C20—C19—C24113.2 (15)
C6—C5—H5119.9C24—C19—P2121.0 (14)
C1—C6—H6119.8C19—C20—H20118.1
C5—C6—C1120.5 (6)C21—C20—C19123.9 (12)
C5—C6—H6119.8C21—C20—H20118.1
C8—C7—P1118.9 (15)C20—C21—H21121.3
C8—C7—C12123.1 (18)C20—C21—C22117.4 (12)
C12—C7—P1118.1 (13)C22—C21—H21121.3
C7—C8—H8120.2C21—C22—H22119.3
C7—C8—C9119.7 (15)C23—C22—C21121.4 (15)
C9—C8—H8120.2C23—C22—H22119.3
C8—C9—H9119.5C22—C23—H23119.2
C10—C9—C8120.9 (14)C22—C23—C24121.6 (16)
C10—C9—H9119.5C24—C23—H23119.2
C9—C10—H10120.2C19—C24—H24118.8
C9—C10—C11119.6 (15)C23—C24—C19122.5 (15)
C11—C10—H10120.2C23—C24—H24118.8
C10—C11—H11120.4C20A—C19A—P2120.4 (12)
C12—C11—C10119.3 (13)C20A—C19A—C24A124.9 (15)
C12—C11—H11120.4C24A—C19A—P2114.5 (12)
C7—C12—C11117.5 (13)C19A—C20A—H20A121.6
C7—C12—H12121.3C19A—C20A—C21A116.9 (13)
C11—C12—H12121.3C21A—C20A—H20A121.6
C8A—C7A—P1120.6 (15)C20A—C21A—H21A119.3
C12A—C7A—P1124.7 (15)C22A—C21A—C20A121.5 (14)
C12A—C7A—C8A114.6 (17)C22A—C21A—H21A119.3
C7A—C8A—H8A119.5C21A—C22A—H22A119.3
C9A—C8A—C7A121.1 (15)C21A—C22A—C23A121.5 (13)
C9A—C8A—H8A119.5C23A—C22A—H22A119.3
C8A—C9A—H9A120.1C22A—C23A—H23A121.3
C8A—C9A—C10A119.8 (13)C24A—C23A—C22A117.3 (12)
C10A—C9A—H9A120.1C24A—C23A—H23A121.3
C9A—C10A—H10A120.0C19A—C24A—C23A117.9 (13)
C11A—C10A—C9A120.1 (14)C19A—C24A—H24A121.1
C11A—C10A—H10A120.0C23A—C24A—H24A121.1
C10A—C11A—H11A119.8
Te1—P1—N1—P29.3 (5)C7—P1—C1—C295.2 (7)
Te1—P1—C1—C2144.2 (4)C7—P1—C1—C682.8 (8)
Te1—P1—C1—C637.9 (5)C7—C8—C9—C100.4 (6)
Te1—P1—C7—C8107.5 (7)C8—C7—C12—C110.7 (11)
Te1—P1—C7—C1270.5 (8)C8—C9—C10—C110.6 (11)
Te1—P1—C7A—C8A144.4 (7)C9—C10—C11—C120.2 (14)
Te1—P1—C7A—C12A38.9 (10)C10—C11—C12—C70.4 (13)
Te2—P2—N1—P167.9 (4)C12—C7—C8—C90.3 (6)
Te2—P2—C13—C1463.3 (17)C7A—P1—N1—P2130.7 (6)
Te2—P2—C13—C18118.0 (15)C7A—P1—C1—C2101.4 (9)
Te2—P2—C13A—C14A76.0 (12)C7A—P1—C1—C676.5 (9)
Te2—P2—C13A—C18A106.4 (15)C7A—C8A—C9A—C10A0.5 (5)
Te2—P2—C19—C202.3 (9)C8A—C7A—C12A—C11A0.5 (11)
Te2—P2—C19—C24179.3 (7)C8A—C9A—C10A—C11A1.5 (11)
P1—C1—C2—C3179.9 (5)C9A—C10A—C11A—C12A2.0 (14)
P1—C1—C6—C5179.2 (5)C10A—C11A—C12A—C7A1.6 (14)
P1—C7—C8—C9178.2 (8)C12A—C7A—C8A—C9A0.0 (5)
P1—C7—C12—C11178.6 (8)C13—P2—N1—P1175.0 (7)
P1—C7A—C8A—C9A177.1 (9)C13—P2—C19—C20107.4 (11)
P1—C7A—C12A—C11A177.4 (9)C13—P2—C19—C2469.6 (11)
P2—C13—C14—C15176.6 (13)C13—C14—C15—C161 (3)
P2—C13—C18—C17175.2 (14)C14—C13—C18—C174 (3)
P2—C13A—C14A—C15A179.4 (11)C14—C15—C16—C173 (2)
P2—C13A—C18A—C17A179.0 (13)C15—C16—C17—C181 (2)
P2—C19—C20—C21177.1 (9)C16—C17—C18—C132 (3)
P2—C19—C24—C23176.7 (9)C18—C13—C14—C152 (3)
P2—C19A—C20A—C21A174.3 (7)C13A—P2—N1—P1174.5 (6)
P2—C19A—C24A—C23A175.1 (8)C13A—C14A—C15A—C16A1 (2)
N1—P1—C1—C216.4 (5)C14A—C13A—C18A—C17A4 (2)
N1—P1—C1—C6165.6 (5)C14A—C15A—C16A—C17A1 (2)
N1—P1—C7—C820.8 (7)C15A—C16A—C17A—C18A0 (2)
N1—P1—C7—C12161.2 (7)C16A—C17A—C18A—C13A3 (2)
N1—P1—C7A—C8A16.9 (8)C18A—C13A—C14A—C15A2 (2)
N1—P1—C7A—C12A166.4 (8)C19—P2—N1—P163.6 (7)
N1—P2—C13—C14170.6 (15)C19—P2—C13—C1454.0 (18)
N1—P2—C13—C188.0 (17)C19—P2—C13—C18124.7 (16)
N1—P2—C13A—C14A159.8 (11)C19—C20—C21—C221.0 (5)
N1—P2—C13A—C18A17.7 (15)C20—C19—C24—C230.7 (11)
N1—P2—C19—C20136.2 (8)C20—C21—C22—C232.7 (12)
N1—P2—C19—C2446.8 (9)C21—C22—C23—C243.5 (16)
C1—P1—N1—P2112.5 (4)C22—C23—C24—C192.4 (15)
C1—P1—C7—C8135.7 (6)C24—C19—C20—C210.1 (5)
C1—P1—C7—C1246.3 (8)C19A—P2—N1—P160.7 (6)
C1—P1—C7A—C8A101.1 (8)C19A—P2—C13A—C14A40.1 (14)
C1—P1—C7A—C12A75.7 (10)C19A—P2—C13A—C18A137.4 (14)
C1—C2—C3—C42.1 (10)C19A—C20A—C21A—C22A1.0 (5)
C2—C1—C6—C51.3 (9)C20A—C19A—C24A—C23A0.5 (11)
C2—C3—C4—C51.3 (11)C20A—C21A—C22A—C23A2.5 (11)
C3—C4—C5—C60.5 (11)C21A—C22A—C23A—C24A2.9 (13)
C4—C5—C6—C10.5 (11)C22A—C23A—C24A—C19A1.8 (12)
C6—C1—C2—C32.1 (9)C24A—C19A—C20A—C21A0.0 (5)
C7—P1—N1—P2134.9 (5)
Symmetry code: (i) x+2, y+1, z.

Experimental details

Crystal data
Chemical formulaC48H40N2P4Te5
Mr1406.70
Crystal system, space groupMonoclinic, P21/c
Temperature (K)173
a, b, c (Å)11.021 (2), 14.950 (3), 15.893 (3)
β (°) 113.47 (3)
V3)2402.2 (10)
Z2
Radiation typeMo Kα
µ (mm1)3.17
Crystal size (mm)0.02 × 0.02 × 0.02
Data collection
DiffractometerNonius KappaCCD
diffractometer
Absorption correctionIntegration
(SCALEPACK; Otwinowski & Minor, 1997)
Tmin, Tmax0.939, 0.939
No. of measured, independent and
observed [I > 2σ(I)] reflections
8246, 4216, 3159
Rint0.033
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.083, 1.08
No. of reflections4216
No. of parameters253
No. of restraints12
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.60, 0.71

Computer programs: COLLECT (Nonius, 2001), DENZO (Nonius, 2001), SHELXS97 (Sheldrick, 2008), SHELXL2014 (Sheldrick, 2008), OLEX2 (Dolomanov et al., 2009).

 

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