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Acta Crystallogr Sect E Struct Rep Online. 2009 September 1; 65(Pt 9): o2214.
Published online 2009 August 22. doi:  10.1107/S1600536809032802
PMCID: PMC2970049

1,1,2,2-Tetra­kis(diisopropyl­amino)diphosphane

Abstract

In the title compound, C24H56N4P2, the distance between the P atoms [2.2988 (8) and 2.3013 (13) Å in the major and minor occupancy components, respectively] is one of the longest reported for uncoordinated diphosphanes. The whole mol­ecule is disordered over two positions with site-occupation factors of 0.6447 (8) and 0.3553 (8). The structure adopts the synperiplanar conformation in the solid state [N—P—P—N torsion angle = 14.7 (5)°].

Related literature

For reactions of diphosphanes with transition metal chlorides, see: Pikies et al. (2004 [triangle]). For related structures, see: Becker et al. (1999 [triangle]); Bezombes et al. (2004 [triangle]); Hinchley et al. (2001 [triangle], 2004 [triangle]); Mundt et al. (1988 [triangle]); Bender et al. (1994 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-o2214-scheme1.jpg

Experimental

Crystal data

  • C24H56N4P2
  • M r = 462.67
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-o2214-efi1.jpg
  • a = 11.601 (2) Å
  • b = 14.493 (3) Å
  • c = 17.280 (4) Å
  • β = 97.22 (3)°
  • V = 2882.2 (10) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 0.17 mm−1
  • T = 150 K
  • 0.38 × 0.23 × 0.21 mm

Data collection

  • Stoe IPDS 2 diffractometer
  • Absorption correction: none
  • 20113 measured reflections
  • 5601 independent reflections
  • 4529 reflections with I > 2σ(I)
  • R int = 0.032

Refinement

  • R[F 2 > 2σ(F 2)] = 0.038
  • wR(F 2) = 0.105
  • S = 1.03
  • 5601 reflections
  • 518 parameters
  • 6 restraints
  • H-atom parameters constrained
  • Δρmax = 0.30 e Å−3
  • Δρmin = −0.17 e Å−3

Data collection: X-AREA (Stoe & Cie, 1997 [triangle]); cell refinement: X-AREA; data reduction: X-RED (Stoe & Cie, 1997 [triangle]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: ORTEP-3 (Farrugia, 1997 [triangle]); software used to prepare material for publication: WinGX32 (Farrugia, 1999 [triangle]).

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809032802/pv2196sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809032802/pv2196Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

supplementary crystallographic information

Comment

In the course of our studies on phosphinophosphinidene ligands R2P–P we have investigated reactions of diphosphanes R2P—P(SiMe3)Li with transition metals chlorides (Pikies et al., 2004). The title compound, (iPr2N)2P–P(NiPr2)2 (I), turned out to be the main product in the reaction of (iPr2N)2P–P(SiMe3)Li with [Cp2ZrCl2] (mol ratio 2:1 in DME); (I) is formed as a result of cleavage of the P–P bond in the starting material, (iPr2N)2P—P(SiMe3)Li. We observed the formation of diphosphanes (R2P–PR2) in every reaction of [Cp2ZrCl2] with R2P—P(SiMe3)Li in different yields. The formation of diphosphane in exceptionally preferred in the case of R=iPr2N. The crystal structure of (I) is presented in this paper.

The whole molecule of the title compound was disordered over two positions with site occupation factors of 0.6447 (8) and 0.3553 (8) referred to as part A and B, respectively; the part A is presented in Fig. 1. The structure adopts the synperiplanar conformation in the solid state (N1—P1—P2—N4 torsion 14.7 (5)°). The most striking structural feature in (I) is P1–P2 bond length (2.2988 (8) Å in part A and 2.3013 (13) Å in part B). This distance between phosphorous atoms is one of the longest reported for uncoordinated diphosphanes. There is only one report of diphoshane {P[CH(SiMe3)2]2}2 with a longer P–P bond of 2.310 (7) Å (Hinchley et al., 2001). Another diphosphane which contains amino grups [N(SiMe3)2](NiPr2)P–P[N(SiMe3)2](NiPr2) has slightly shorter P–P distance of 2.291 (4) Å (Bezombes et al., 2004). These three diphosphanes R2P–PR2 posses R groups which have a form of –AX2, where A = N or CH and X are voluminous rests SiMe3 or iPr. The steric effects of bulky R groups like tBu are not sufficient for such an elongation (Hinchley et al., 2004) and for tBu2P–PtBu2 a P–P distance of 2.235 Å was reported. The presence of four nitrogen substituents in the molecule is not sufficient cause of the elongation either. For DMP(iPr2N)P–P(NiPr2)DMP (DMP = 2,6-dimethylopiperidine) the P–P distance of 2.259 (2) Å was reported (Bender et al., 1994). The enhanced stabilities of related radicals P[CH(SiMe3)2] or P[N(SiMe3)2](NiPr2) can be seen as a possible explanation of the elongation phenomena. These diphosphanes dissociate very easy into relatively stable radicals (Hinchley et al., 2001).

To study repulsions of substituents around P-atom we analysed the average angle around P atoms. Its deviation from orthogonality (90°) can be a rough measure of the steric crowding. The average angle in (I) around P atoms is 105.98°. The widest ones, above 110°, are N—P—P angles for N1 and N4 (in disorder part A), perhaps because nitrogen atoms are in synperiplanar position. The N—P—P angles for N3 and N2 atoms are only 93.5 (6)° and 92.0 (4)°, respectively. For comparison, in the case of very small groups around P-atoms, i.e., for Me2P–PMe2 the average angle is 98.40° (close to orthogonality) (Mundt et al., 1988) and for (F3C)2P–P(CF3)2 is only 96.67° (Becker et al., 1999). For the most crowded diphosphanes, i.e., for tBu2P–PtBu2, this average angle is 109.99° (Hinchley et al., 2004) and for [(Me3Si)2CH]2P–P[CH(SiMe3)2]2 is 105.23° (Hinchley et al., 2001).

Experimental

The work was carried out using the standard vacuum-nitrogen line and Schlenk techniques. Solution of 0.244 g (0.447 mmol) (iPr2N)2P—P(SiMe3)Li . 2.6THF in 2 ml DME was added dropwise into solution of 0.059 g (0.202 mmol) [Cp2ZrCl2] in 2 ml of DME at 233 K. The mixture immediately turned red. The resultant solution was studied using 31P-NMR. Then the volume was reduced to about 2 ml and the concentrate stored for 3 days at 269 K. After this time the solution yielded small colourless crystals of (I).

Refinement

All H atoms were placed in calculated positions and refined as riding on their carrier atoms with respective Uiso(H) values: C—H = 0.98 Å (CH3) and Uiso(H) = 1.5 Ueq(C), C—H = 1.00 Å (CH) and Uĩso(H) = 1.2 Ueq(C). The whole molecule was refined as disordered over two positions with site occupation factors of 0.6447 (8) / 0.3553 (8). Additionally, P–N bond lengths were restrained to be the same and all N atoms displacement ellipsoids were restrained to be equal to improve numerical stability. This kind of disorder was noted already for the structurally similar {P[N(SiMe3)2](NiPr2)2 (Bezombes et al., 2004).

Figures

Fig. 1.
View of (I) (50% probability displacement ellipsoids), hydrogen atoms omitted. Only the more occupated part shown.
Fig. 2.
Jmol enhanced figure. Disorder in (I).

Crystal data

C24H56N4P2F(000) = 1032
Mr = 462.67Dx = 1.066 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 18348 reflections
a = 11.601 (2) Åθ = 3.9–51.8°
b = 14.493 (3) ŵ = 0.17 mm1
c = 17.280 (4) ÅT = 150 K
β = 97.22 (3)°Block, colourless
V = 2882.2 (10) Å30.38 × 0.23 × 0.21 mm
Z = 4

Data collection

Stoe IPDS 2 diffractometer4529 reflections with I > 2σ(I)
graphiteRint = 0.032
Detector resolution: 6.67 pixels mm-1θmax = 26.0°, θmin = 1.8°
rotation scansh = −14→14
20113 measured reflectionsk = −17→16
5601 independent reflectionsl = −21→21

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.105H-atom parameters constrained
S = 1.03w = 1/[σ2(Fo2) + (0.0687P)2 + 0.2046P] where P = (Fo2 + 2Fc2)/3
5601 reflections(Δ/σ)max = 0.001
518 parametersΔρmax = 0.30 e Å3
6 restraintsΔρmin = −0.16 e Å3

Special details

Experimental. 31P{1H} NMR (162 MHz, external standard 85% H3PO4) of (I) (THF, C6D6): 83 p.p.m. (s)
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.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/UeqOcc. (<1)
N10.2977 (8)0.7824 (6)0.1952 (4)0.0238 (8)0.6447 (8)
N20.4712 (13)0.7701 (7)0.3244 (7)0.0260 (10)0.6447 (8)
N30.6486 (10)0.8478 (11)0.1705 (6)0.0279 (12)0.6447 (8)
N40.5268 (16)0.6946 (7)0.0985 (5)0.0255 (11)0.6447 (8)
P10.42982 (4)0.81988 (3)0.23709 (3)0.02262 (14)0.6447 (8)
P20.57580 (4)0.74749 (3)0.18190 (3)0.02261 (14)0.6447 (8)
C10.2484 (2)0.68862 (15)0.21064 (12)0.0281 (4)0.6447 (8)
H1A0.31480.64910.23350.034*0.6447 (8)
C20.1612 (8)0.6905 (7)0.2688 (6)0.0435 (17)0.6447 (8)
H2A0.19490.72290.31610.065*0.6447 (8)
H2B0.14160.62720.28210.065*0.6447 (8)
H2C0.09080.72270.2460.065*0.6447 (8)
C30.1894 (7)0.6384 (7)0.1372 (4)0.0425 (15)0.6447 (8)
H3A0.24420.6340.09850.064*0.6447 (8)
H3B0.12060.67320.1150.064*0.6447 (8)
H3C0.16610.57630.15140.064*0.6447 (8)
C40.2107 (2)0.85070 (18)0.16444 (15)0.0321 (5)0.6447 (8)
H4A0.14070.81590.14060.039*0.6447 (8)
C50.2529 (4)0.9089 (3)0.0997 (3)0.0398 (9)0.6447 (8)
H5A0.29830.87020.06830.06*0.6447 (8)
H5B0.30170.95940.1230.06*0.6447 (8)
H5C0.18590.93450.06650.06*0.6447 (8)
C60.1714 (8)0.9144 (6)0.2269 (6)0.049 (2)0.6447 (8)
H6A0.11540.95940.20220.074*0.6447 (8)
H6B0.23890.9470.25380.074*0.6447 (8)
H6C0.13480.87760.26470.074*0.6447 (8)
C70.4946 (2)0.67694 (16)0.34661 (14)0.0318 (5)0.6447 (8)
H7A0.48280.63980.29750.038*0.6447 (8)
C80.4196 (10)0.6315 (7)0.4033 (5)0.0458 (14)0.6447 (8)
H8A0.33820.64960.38940.069*0.6447 (8)
H8B0.44650.65160.45660.069*0.6447 (8)
H8C0.42620.56420.39990.069*0.6447 (8)
C90.6208 (6)0.6637 (5)0.3806 (3)0.0478 (14)0.6447 (8)
H9A0.67140.69260.34630.072*0.6447 (8)
H9B0.63820.59760.38510.072*0.6447 (8)
H9C0.63420.69230.43240.072*0.6447 (8)
C100.4729 (2)0.83599 (18)0.39749 (15)0.0366 (5)0.6447 (8)
H10A0.50280.79820.44410.044*0.6447 (8)
C110.3567 (11)0.8734 (7)0.4129 (5)0.059 (3)0.6447 (8)
H11A0.30160.82230.41420.088*0.6447 (8)
H11B0.32760.91650.37130.088*0.6447 (8)
H11C0.36530.90560.46320.088*0.6447 (8)
C120.5594 (10)0.9140 (8)0.3935 (6)0.049 (3)0.6447 (8)
H12A0.55810.95450.43870.073*0.6447 (8)
H12B0.53830.94940.34550.073*0.6447 (8)
H12C0.63750.88830.39360.073*0.6447 (8)
C130.7796 (2)0.8453 (2)0.18204 (14)0.0358 (5)0.6447 (8)
H13A0.8060.91060.17790.043*0.6447 (8)
C140.8195 (6)0.8155 (8)0.2632 (6)0.050 (2)0.6447 (8)
H14A0.90460.81590.2720.075*0.6447 (8)
H14B0.7910.75310.27130.075*0.6447 (8)
H14C0.78910.8580.29980.075*0.6447 (8)
C150.8412 (9)0.7908 (7)0.1267 (4)0.055 (2)0.6447 (8)
H15A0.81530.8110.07320.083*0.6447 (8)
H15B0.82350.72510.13190.083*0.6447 (8)
H15C0.92510.80050.13850.083*0.6447 (8)
C160.6009 (3)0.93370 (19)0.13371 (16)0.0316 (6)0.6447 (8)
H16A0.5150.92440.12220.038*0.6447 (8)
C170.6190 (3)1.0128 (3)0.1930 (2)0.0440 (8)0.6447 (8)
H17A0.59390.9930.24240.066*0.6447 (8)
H17B0.57321.06640.17290.066*0.6447 (8)
H17C0.70151.02940.20150.066*0.6447 (8)
C180.6440 (6)0.9630 (6)0.0552 (5)0.048 (2)0.6447 (8)
H18A0.63040.91260.01740.073*0.6447 (8)
H18B0.72730.97690.06430.073*0.6447 (8)
H18C0.60141.0180.03470.073*0.6447 (8)
C190.48180 (18)0.74866 (17)0.02342 (11)0.0287 (4)0.6447 (8)
H19A0.47580.81480.03880.034*0.6447 (8)
C200.5698 (9)0.7446 (6)−0.0384 (4)0.053 (2)0.6447 (8)
H20A0.64710.7631−0.01380.079*0.6447 (8)
H20B0.54420.7867−0.08150.079*0.6447 (8)
H20C0.57320.6815−0.05840.079*0.6447 (8)
C210.3607 (8)0.7197 (4)−0.0162 (5)0.0397 (12)0.6447 (8)
H21A0.3050.72190.02190.059*0.6447 (8)
H21B0.36450.6567−0.03640.059*0.6447 (8)
H21C0.33580.762−0.05930.059*0.6447 (8)
C220.5456 (2)0.59768 (15)0.08539 (16)0.0317 (5)0.6447 (8)
H22A0.50890.58080.03180.038*0.6447 (8)
C230.6843 (6)0.5780 (5)0.0923 (4)0.061 (2)0.6447 (8)
H23A0.72610.63680.09210.091*0.6447 (8)
H23B0.70120.54040.0480.091*0.6447 (8)
H23C0.70940.54510.14110.091*0.6447 (8)
C240.4973 (9)0.5405 (8)0.1416 (6)0.047 (2)0.6447 (8)
H24A0.4150.55560.14170.071*0.6447 (8)
H24B0.53930.55160.19360.071*0.6447 (8)
H24C0.50490.47540.12770.071*0.6447 (8)
N1A0.2873 (15)0.7756 (13)0.2098 (9)0.0238 (8)0.3553 (8)
N2A0.467 (3)0.7837 (15)0.3328 (14)0.0260 (10)0.3553 (8)
N3A0.6421 (19)0.843 (2)0.1580 (13)0.0279 (12)0.3553 (8)
N4A0.522 (3)0.7000 (13)0.0864 (10)0.0255 (11)0.3553 (8)
P1A0.42218 (7)0.73311 (6)0.23673 (5)0.0219 (2)0.3553 (8)
P2A0.50767 (7)0.79679 (6)0.13605 (5)0.0230 (2)0.3553 (8)
C1A0.1834 (4)0.7206 (3)0.2072 (3)0.0344 (9)0.3553 (8)
H1B0.11610.76380.19630.041*0.3553 (8)
C2A0.1744 (14)0.6767 (14)0.2854 (12)0.060 (4)0.3553 (8)
H2D0.18480.7240.32620.09*0.3553 (8)
H2E0.23480.62950.2960.09*0.3553 (8)
H2F0.09770.64820.28480.09*0.3553 (8)
C3A0.1765 (13)0.6541 (12)0.1395 (10)0.050 (4)0.3553 (8)
H3D0.18060.68850.09110.075*0.3553 (8)
H3E0.10290.62020.13570.075*0.3553 (8)
H3F0.24140.61050.14780.075*0.3553 (8)
C4A0.2637 (4)0.8765 (3)0.1849 (3)0.0301 (9)0.3553 (8)
H4B0.34050.90870.190.036*0.3553 (8)
C5A0.2117 (6)0.8852 (6)0.1017 (5)0.0424 (16)0.3553 (8)
H5D0.24430.83750.07050.064*0.3553 (8)
H5E0.22960.94630.0820.064*0.3553 (8)
H5F0.12730.87740.09790.064*0.3553 (8)
C6A0.1864 (13)0.9294 (11)0.2368 (11)0.040 (3)0.3553 (8)
H6D0.19320.90080.28850.061*0.3553 (8)
H6E0.10530.9270.21280.061*0.3553 (8)
H6F0.21180.99390.24180.061*0.3553 (8)
C7A0.5286 (4)0.7087 (3)0.3852 (3)0.0345 (9)0.3553 (8)
H7B0.56690.7420.43230.041*0.3553 (8)
C8A0.4313 (18)0.6493 (12)0.4147 (11)0.062 (5)0.3553 (8)
H8D0.46640.60390.45260.093*0.3553 (8)
H8E0.38750.61730.37050.093*0.3553 (8)
H8F0.37880.68940.43960.093*0.3553 (8)
C9A0.6228 (12)0.6495 (9)0.3576 (5)0.046 (2)0.3553 (8)
H9D0.65470.60810.39970.069*0.3553 (8)
H9E0.68490.68920.34280.069*0.3553 (8)
H9F0.58990.6130.31240.069*0.3553 (8)
C10A0.4613 (3)0.8703 (3)0.3545 (3)0.0276 (8)0.3553 (8)
H10B0.42260.9060.3090.033*0.3553 (8)
C11A0.3793 (19)0.8709 (11)0.4182 (9)0.040 (3)0.3553 (8)
H11D0.37530.93340.43930.059*0.3553 (8)
H11E0.40890.82840.46010.059*0.3553 (8)
H11F0.30140.85130.39550.059*0.3553 (8)
C12A0.5729 (16)0.9193 (11)0.3839 (10)0.038 (3)0.3553 (8)
H12D0.63250.90370.35050.057*0.3553 (8)
H12E0.5990.89990.43750.057*0.3553 (8)
H12F0.55970.98610.38260.057*0.3553 (8)
C13A0.7460 (4)0.7966 (4)0.1930 (2)0.0372 (9)0.3553 (8)
H13B0.72280.7310.20.045*0.3553 (8)
C14A0.8154 (13)0.8268 (14)0.2733 (12)0.052 (4)0.3553 (8)
H14D0.76640.81850.3150.078*0.3553 (8)
H14E0.83760.89180.27060.078*0.3553 (8)
H14F0.88550.78880.28420.078*0.3553 (8)
C15A0.8263 (18)0.7953 (13)0.1260 (10)0.062 (4)0.3553 (8)
H15D0.78320.76950.07850.094*0.3553 (8)
H15E0.89490.75720.14210.094*0.3553 (8)
H15F0.85070.85840.11580.094*0.3553 (8)
C16A0.6525 (5)0.9454 (4)0.1463 (3)0.0403 (13)0.3553 (8)
H16B0.73150.9640.17130.048*0.3553 (8)
C17A0.5667 (6)1.0084 (5)0.1782 (6)0.0556 (19)0.3553 (8)
H17D0.57040.99920.23460.083*0.3553 (8)
H17E0.48820.99430.15310.083*0.3553 (8)
H17F0.58571.07270.16750.083*0.3553 (8)
C18A0.6494 (12)0.9617 (8)0.0615 (8)0.043 (4)0.3553 (8)
H18D0.70250.91870.04020.064*0.3553 (8)
H18E0.67351.02520.05260.064*0.3553 (8)
H18F0.57020.95190.03570.064*0.3553 (8)
C19A0.4963 (4)0.6847 (4)0.0071 (2)0.0381 (10)0.3553 (8)
H19B0.52010.6204−0.00460.046*0.3553 (8)
C20A0.5551 (16)0.7475 (9)−0.0386 (8)0.048 (4)0.3553 (8)
H20D0.63910.7435−0.02260.073*0.3553 (8)
H20E0.52860.8106−0.03040.073*0.3553 (8)
H20F0.5380.7314−0.09390.073*0.3553 (8)
C21A0.3689 (15)0.6925 (9)−0.0127 (8)0.054 (3)0.3553 (8)
H21D0.33060.64680.01730.081*0.3553 (8)
H21E0.34780.6812−0.06860.081*0.3553 (8)
H21F0.34390.75460.00020.081*0.3553 (8)
C22A0.5765 (4)0.6081 (3)0.1319 (3)0.0368 (9)0.3553 (8)
H22B0.60750.6250.18670.044*0.3553 (8)
C23A0.6722 (10)0.5668 (9)0.0927 (5)0.039 (2)0.3553 (8)
H23D0.69780.61140.05580.059*0.3553 (8)
H23E0.64380.51090.06460.059*0.3553 (8)
H23F0.73760.5510.1320.059*0.3553 (8)
C24A0.4815 (16)0.5278 (14)0.1335 (8)0.037 (3)0.3553 (8)
H24D0.51870.47260.15820.056*0.3553 (8)
H24E0.44790.51310.08010.056*0.3553 (8)
H24F0.41990.54860.16340.056*0.3553 (8)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
N10.0217 (17)0.0209 (15)0.030 (3)−0.0036 (11)0.0062 (16)0.0064 (17)
N20.0463 (13)0.015 (3)0.016 (3)0.001 (2)0.0028 (16)−0.0104 (16)
N30.0247 (14)0.0365 (16)0.021 (4)−0.0063 (7)−0.0041 (19)0.001 (2)
N40.0359 (15)0.0289 (12)0.010 (3)0.0046 (11)−0.003 (3)0.0028 (18)
P10.0260 (3)0.0206 (3)0.0218 (2)−0.00339 (18)0.00516 (18)−0.00181 (18)
P20.0209 (2)0.0270 (3)0.0196 (2)−0.00019 (18)0.00114 (17)0.00094 (19)
C10.0245 (11)0.0260 (10)0.0343 (11)−0.0034 (9)0.0053 (9)−0.0004 (8)
C20.041 (2)0.0459 (19)0.045 (5)−0.0078 (14)0.011 (2)0.004 (2)
C30.048 (3)0.031 (2)0.043 (3)−0.0070 (19)−0.014 (2)−0.0052 (19)
C40.0259 (12)0.0292 (12)0.0418 (14)0.0054 (10)0.0068 (10)0.0003 (11)
C50.047 (2)0.036 (2)0.0387 (15)0.0144 (14)0.0125 (18)0.0133 (14)
C60.066 (4)0.033 (3)0.053 (4)0.022 (2)0.025 (3)0.010 (3)
C70.0427 (13)0.0284 (12)0.0230 (11)−0.0054 (9)−0.0011 (9)0.0012 (9)
C80.065 (2)0.038 (3)0.0368 (19)−0.009 (2)0.0171 (18)0.0101 (19)
C90.046 (2)0.060 (3)0.034 (3)−0.005 (2)−0.005 (2)0.014 (2)
C100.0535 (15)0.0348 (13)0.0228 (11)−0.0129 (11)0.0095 (10)−0.0068 (10)
C110.059 (5)0.072 (4)0.052 (4)−0.018 (3)0.034 (4)−0.035 (3)
C120.052 (4)0.055 (4)0.042 (3)−0.016 (2)0.017 (2)−0.019 (2)
C130.0208 (11)0.0495 (15)0.0362 (12)−0.0068 (11)0.0004 (9)0.0027 (11)
C140.026 (2)0.086 (5)0.038 (3)−0.016 (2)−0.0001 (18)−0.001 (3)
C150.021 (3)0.107 (5)0.038 (3)−0.001 (3)0.0052 (18)−0.013 (3)
C160.0304 (15)0.0325 (13)0.0316 (13)−0.0086 (12)0.0023 (12)0.0055 (10)
C170.053 (2)0.0352 (15)0.0456 (17)−0.0131 (18)0.0123 (18)0.0014 (12)
C180.041 (3)0.065 (5)0.043 (3)−0.007 (3)0.015 (3)0.026 (3)
C190.0316 (10)0.0341 (12)0.0204 (9)0.0028 (9)0.0028 (8)−0.0007 (9)
C200.050 (3)0.088 (5)0.024 (3)0.005 (2)0.017 (2)0.011 (2)
C210.037 (2)0.045 (2)0.033 (2)0.0051 (19)−0.0103 (15)−0.0037 (15)
C220.0362 (12)0.0302 (11)0.0292 (12)0.0067 (9)0.0060 (10)−0.0051 (10)
C230.054 (3)0.033 (2)0.103 (5)0.027 (2)0.039 (3)0.009 (2)
C240.049 (3)0.020 (3)0.075 (4)0.003 (3)0.011 (2)−0.005 (2)
N1A0.0217 (17)0.0209 (15)0.030 (3)−0.0036 (11)0.0062 (16)0.0064 (17)
N2A0.0463 (13)0.015 (3)0.016 (3)0.001 (2)0.0028 (16)−0.0104 (16)
N3A0.0247 (14)0.0365 (16)0.021 (4)−0.0063 (7)−0.0041 (19)0.001 (2)
N4A0.0359 (15)0.0289 (12)0.010 (3)0.0046 (11)−0.003 (3)0.0028 (18)
P1A0.0230 (4)0.0213 (5)0.0216 (4)0.0007 (3)0.0034 (3)−0.0019 (3)
P2A0.0206 (4)0.0281 (5)0.0202 (4)0.0022 (3)0.0020 (3)0.0014 (3)
C1A0.023 (2)0.035 (2)0.047 (3)−0.0046 (18)0.0092 (17)−0.0086 (19)
C2A0.041 (6)0.103 (11)0.041 (7)−0.033 (6)0.024 (5)−0.003 (6)
C3A0.046 (5)0.037 (6)0.070 (6)−0.021 (5)0.023 (4)−0.018 (4)
C4A0.027 (2)0.028 (2)0.035 (2)0.0026 (17)0.0018 (18)−0.0026 (17)
C5A0.047 (4)0.046 (4)0.034 (3)0.014 (3)0.005 (3)0.004 (3)
C6A0.033 (3)0.042 (5)0.048 (4)0.011 (3)0.011 (3)−0.017 (4)
C7A0.042 (2)0.034 (2)0.027 (2)0.0029 (19)0.0016 (18)0.0029 (18)
C8A0.079 (8)0.043 (7)0.066 (9)0.008 (6)0.014 (5)0.030 (6)
C9A0.061 (4)0.047 (4)0.028 (5)0.029 (3)−0.003 (4)0.010 (3)
C10A0.0306 (19)0.0257 (19)0.026 (2)−0.0025 (15)0.0035 (15)−0.0066 (17)
C11A0.047 (7)0.036 (4)0.035 (4)−0.002 (3)0.001 (4)−0.007 (3)
C12A0.040 (5)0.031 (4)0.038 (5)−0.014 (4)−0.014 (5)−0.011 (4)
C13A0.026 (2)0.053 (3)0.032 (2)0.001 (2)0.0030 (17)0.001 (2)
C14A0.056 (6)0.056 (5)0.035 (5)0.000 (4)−0.027 (4)−0.003 (4)
C15A0.017 (5)0.077 (7)0.091 (9)0.008 (4)0.002 (4)0.018 (6)
C16A0.031 (3)0.044 (3)0.044 (3)−0.012 (3)0.000 (3)0.008 (2)
C17A0.063 (5)0.027 (3)0.080 (5)−0.009 (4)0.022 (4)0.009 (3)
C18A0.056 (7)0.029 (6)0.037 (5)−0.017 (4)−0.016 (4)−0.001 (4)
C19A0.040 (2)0.053 (3)0.0205 (18)0.007 (2)0.0033 (16)−0.0064 (19)
C20A0.057 (7)0.047 (6)0.040 (7)−0.014 (4)0.002 (4)−0.017 (4)
C21A0.040 (4)0.100 (10)0.021 (3)0.022 (6)−0.002 (2)−0.001 (5)
C22A0.042 (2)0.039 (2)0.030 (2)0.0147 (19)0.0054 (19)−0.0013 (19)
C23A0.035 (4)0.053 (5)0.032 (4)−0.012 (3)0.011 (3)−0.009 (3)
C24A0.048 (5)0.027 (6)0.038 (4)−0.010 (3)0.013 (3)0.000 (3)

Geometric parameters (Å, °)

N1—C41.465 (10)N1A—C1A1.441 (17)
N1—C11.512 (8)N1A—C4A1.539 (18)
N1—P11.699 (9)N1A—P1A1.692 (19)
N2—C71.420 (12)N2A—C10A1.313 (19)
N2—C101.582 (7)N2A—C7A1.53 (3)
N2—P11.687 (14)N2A—P1A1.83 (2)
N3—C161.474 (17)N3A—C13A1.45 (3)
N3—C131.508 (12)N3A—C16A1.50 (3)
N3—P21.705 (11)N3A—P2A1.697 (14)
N4—C221.444 (9)N4A—C19A1.383 (17)
N4—C191.549 (10)N4A—C22A1.63 (2)
N4—P21.667 (8)N4A—P2A1.664 (14)
P1—P22.2988 (8)P1A—P2A2.3013 (13)
C1—C21.513 (10)C1A—C2A1.509 (18)
C1—C31.546 (8)C1A—C3A1.510 (18)
C1—H1A1C1A—H1B1
C2—H2A0.98C2A—H2D0.98
C2—H2B0.98C2A—H2E0.98
C2—H2C0.98C2A—H2F0.98
C3—H3A0.98C3A—H3D0.98
C3—H3B0.98C3A—H3E0.98
C3—H3C0.98C3A—H3F0.98
C4—C51.530 (4)C4A—C5A1.494 (10)
C4—C61.533 (10)C4A—C6A1.548 (17)
C4—H4A1C4A—H4B1
C5—H5A0.98C5A—H5D0.98
C5—H5B0.98C5A—H5E0.98
C5—H5C0.98C5A—H5F0.98
C6—H6A0.98C6A—H6D0.98
C6—H6B0.98C6A—H6E0.98
C6—H6C0.98C6A—H6F0.98
C7—C91.520 (7)C7A—C9A1.513 (12)
C7—C81.537 (10)C7A—C8A1.56 (2)
C7—H7A1C7A—H7B1
C8—H8A0.98C8A—H8D0.98
C8—H8B0.98C8A—H8E0.98
C8—H8C0.98C8A—H8F0.98
C9—H9A0.98C9A—H9D0.98
C9—H9B0.98C9A—H9E0.98
C9—H9C0.98C9A—H9F0.98
C10—C111.508 (12)C10A—C12A1.507 (17)
C10—C121.518 (12)C10A—C11A1.54 (2)
C10—H10A1C10A—H10B1
C11—H11A0.98C11A—H11D0.98
C11—H11B0.98C11A—H11E0.98
C11—H11C0.98C11A—H11F0.98
C12—H12A0.98C12A—H12D0.98
C12—H12B0.98C12A—H12E0.98
C12—H12C0.98C12A—H12F0.98
C13—C141.484 (10)C13A—C15A1.574 (18)
C13—C151.490 (9)C13A—C14A1.58 (2)
C13—H13A1C13A—H13B1
C14—H14A0.98C14A—H14D0.98
C14—H14B0.98C14A—H14E0.98
C14—H14C0.98C14A—H14F0.98
C15—H15A0.98C15A—H15D0.98
C15—H15B0.98C15A—H15E0.98
C15—H15C0.98C15A—H15F0.98
C16—C171.534 (5)C16A—C18A1.479 (15)
C16—C181.562 (7)C16A—C17A1.505 (11)
C16—H16A1C16A—H16B1
C17—H17A0.98C17A—H17D0.98
C17—H17B0.98C17A—H17E0.98
C17—H17C0.98C17A—H17F0.98
C18—H18A0.98C18A—H18D0.98
C18—H18B0.98C18A—H18E0.98
C18—H18C0.98C18A—H18F0.98
C19—C211.541 (9)C19A—C20A1.432 (15)
C19—C201.569 (9)C19A—C21A1.478 (17)
C19—H19A1C19A—H19B1
C20—H20A0.98C20A—H20D0.98
C20—H20B0.98C20A—H20E0.98
C20—H20C0.98C20A—H20F0.98
C21—H21A0.98C21A—H21D0.98
C21—H21B0.98C21A—H21E0.98
C21—H21C0.98C21A—H21F0.98
C22—C241.442 (10)C22A—C23A1.496 (12)
C22—C231.624 (7)C22A—C24A1.61 (2)
C22—H22A1C22A—H22B1
C23—H23A0.98C23A—H23D0.98
C23—H23B0.98C23A—H23E0.98
C23—H23C0.98C23A—H23F0.98
C24—H24A0.98C24A—H24D0.98
C24—H24B0.98C24A—H24E0.98
C24—H24C0.98C24A—H24F0.98
C4—N1—C1114.3 (6)C1A—N1A—C4A113.4 (12)
C4—N1—P1118.8 (6)C1A—N1A—P1A123.3 (11)
C1—N1—P1123.6 (6)C4A—N1A—P1A123.3 (10)
C7—N2—C10112.0 (9)C10A—N2A—C7A122.9 (17)
C7—N2—P1132.2 (6)C10A—N2A—P1A128.6 (19)
C10—N2—P1115.4 (7)C7A—N2A—P1A108.0 (10)
C16—N3—C13113.3 (6)C13A—N3A—C16A116.1 (9)
C16—N3—P2127.2 (7)C13A—N3A—P2A127.1 (18)
C13—N3—P2118.0 (11)C16A—N3A—P2A117 (2)
C22—N4—C19113.7 (5)C19A—N4A—C22A111.7 (10)
C22—N4—P2122.8 (7)C19A—N4A—P2A128.5 (15)
C19—N4—P2122.3 (6)C22A—N4A—P2A119.8 (11)
N2—P1—N1112.6 (5)N1A—P1A—N2A104.5 (10)
N2—P1—P292.0 (4)N1A—P1A—P2A96.7 (4)
N1—P1—P2110.4 (3)N2A—P1A—P2A115.2 (9)
N4—P2—N3114.3 (6)N4A—P2A—N3A107.5 (18)
N4—P2—P1112.3 (6)N4A—P2A—P1A97.6 (10)
N3—P2—P193.5 (6)N3A—P2A—P1A117.5 (8)
N1—C1—C2113.6 (5)N1A—C1A—C2A110.9 (9)
N1—C1—C3114.6 (5)N1A—C1A—C3A109.9 (9)
C2—C1—C3106.9 (5)C2A—C1A—C3A114.9 (11)
N1—C1—H1A107.1N1A—C1A—H1B106.9
C2—C1—H1A107.1C2A—C1A—H1B106.9
C3—C1—H1A107.1C3A—C1A—H1B106.9
C1—C2—H2A109.5C1A—C2A—H2D109.5
C1—C2—H2B109.5C1A—C2A—H2E109.5
H2A—C2—H2B109.5H2D—C2A—H2E109.5
C1—C2—H2C109.5C1A—C2A—H2F109.5
H2A—C2—H2C109.5H2D—C2A—H2F109.5
H2B—C2—H2C109.5H2E—C2A—H2F109.5
C1—C3—H3A109.5C1A—C3A—H3D109.5
C1—C3—H3B109.5C1A—C3A—H3E109.5
H3A—C3—H3B109.5H3D—C3A—H3E109.5
C1—C3—H3C109.5C1A—C3A—H3F109.5
H3A—C3—H3C109.5H3D—C3A—H3F109.5
H3B—C3—H3C109.5H3E—C3A—H3F109.5
N1—C4—C5111.6 (3)C5A—C4A—N1A112.6 (8)
N1—C4—C6113.8 (5)C5A—C4A—C6A108.8 (8)
C5—C4—C6109.5 (4)N1A—C4A—C6A113.9 (9)
N1—C4—H4A107.2C5A—C4A—H4B107
C5—C4—H4A107.2N1A—C4A—H4B107
C6—C4—H4A107.2C6A—C4A—H4B107
C4—C5—H5A109.5C4A—C5A—H5D109.5
C4—C5—H5B109.5C4A—C5A—H5E109.5
H5A—C5—H5B109.5H5D—C5A—H5E109.5
C4—C5—H5C109.5C4A—C5A—H5F109.5
H5A—C5—H5C109.5H5D—C5A—H5F109.5
H5B—C5—H5C109.5H5E—C5A—H5F109.5
C4—C6—H6A109.5C4A—C6A—H6D109.5
C4—C6—H6B109.5C4A—C6A—H6E109.5
H6A—C6—H6B109.5H6D—C6A—H6E109.5
C4—C6—H6C109.5C4A—C6A—H6F109.5
H6A—C6—H6C109.5H6D—C6A—H6F109.5
H6B—C6—H6C109.5H6E—C6A—H6F109.5
N2—C7—C9111.5 (7)C9A—C7A—N2A121.2 (9)
N2—C7—C8118.4 (7)C9A—C7A—C8A111.9 (9)
C9—C7—C8107.1 (5)N2A—C7A—C8A106.2 (13)
N2—C7—H7A106.4C9A—C7A—H7B105.4
C9—C7—H7A106.4N2A—C7A—H7B105.4
C8—C7—H7A106.4C8A—C7A—H7B105.4
C7—C8—H8A109.5C7A—C8A—H8D109.5
C7—C8—H8B109.5C7A—C8A—H8E109.5
H8A—C8—H8B109.5H8D—C8A—H8E109.5
C7—C8—H8C109.5C7A—C8A—H8F109.5
H8A—C8—H8C109.5H8D—C8A—H8F109.5
H8B—C8—H8C109.5H8E—C8A—H8F109.5
C7—C9—H9A109.5C7A—C9A—H9D109.5
C7—C9—H9B109.5C7A—C9A—H9E109.5
H9A—C9—H9B109.5H9D—C9A—H9E109.5
C7—C9—H9C109.5C7A—C9A—H9F109.5
H9A—C9—H9C109.5H9D—C9A—H9F109.5
H9B—C9—H9C109.5H9E—C9A—H9F109.5
C11—C10—C12110.6 (7)N2A—C10A—C12A118.5 (15)
C11—C10—N2115.9 (7)N2A—C10A—C11A105.4 (14)
C12—C10—N2110.8 (7)C12A—C10A—C11A109.8 (11)
C11—C10—H10A106.3N2A—C10A—H10B107.6
C12—C10—H10A106.3C12A—C10A—H10B107.6
N2—C10—H10A106.3C11A—C10A—H10B107.6
C10—C11—H11A109.5C10A—C11A—H11D109.5
C10—C11—H11B109.5C10A—C11A—H11E109.5
H11A—C11—H11B109.5H11D—C11A—H11E109.5
C10—C11—H11C109.5C10A—C11A—H11F109.5
H11A—C11—H11C109.5H11D—C11A—H11F109.5
H11B—C11—H11C109.5H11E—C11A—H11F109.5
C10—C12—H12A109.5C10A—C12A—H12D109.5
C10—C12—H12B109.5C10A—C12A—H12E109.5
H12A—C12—H12B109.5H12D—C12A—H12E109.5
C10—C12—H12C109.5C10A—C12A—H12F109.5
H12A—C12—H12C109.5H12D—C12A—H12F109.5
H12B—C12—H12C109.5H12E—C12A—H12F109.5
C14—C13—C15109.6 (6)N3A—C13A—C15A103.8 (12)
C14—C13—N3108.7 (5)N3A—C13A—C14A123.0 (13)
C15—C13—N3119.0 (6)C15A—C13A—C14A111.5 (10)
C14—C13—H13A106.3N3A—C13A—H13B105.8
C15—C13—H13A106.3C15A—C13A—H13B105.8
N3—C13—H13A106.3C14A—C13A—H13B105.8
C13—C14—H14A109.5C13A—C14A—H14D109.5
C13—C14—H14B109.5C13A—C14A—H14E109.5
H14A—C14—H14B109.5H14D—C14A—H14E109.5
C13—C14—H14C109.5C13A—C14A—H14F109.5
H14A—C14—H14C109.5H14D—C14A—H14F109.5
H14B—C14—H14C109.5H14E—C14A—H14F109.5
C13—C15—H15A109.5C13A—C15A—H15D109.5
C13—C15—H15B109.5C13A—C15A—H15E109.5
H15A—C15—H15B109.5H15D—C15A—H15E109.5
C13—C15—H15C109.5C13A—C15A—H15F109.5
H15A—C15—H15C109.5H15D—C15A—H15F109.5
H15B—C15—H15C109.5H15E—C15A—H15F109.5
N3—C16—C17109.3 (5)C18A—C16A—N3A107.3 (11)
N3—C16—C18117.4 (6)C18A—C16A—C17A109.3 (8)
C17—C16—C18110.2 (4)N3A—C16A—C17A118.8 (11)
N3—C16—H16A106.4C18A—C16A—H16B106.9
C17—C16—H16A106.4N3A—C16A—H16B106.9
C18—C16—H16A106.4C17A—C16A—H16B106.9
C16—C17—H17A109.5C16A—C17A—H17D109.5
C16—C17—H17B109.5C16A—C17A—H17E109.5
H17A—C17—H17B109.5H17D—C17A—H17E109.5
C16—C17—H17C109.5C16A—C17A—H17F109.5
H17A—C17—H17C109.5H17D—C17A—H17F109.5
H17B—C17—H17C109.5H17E—C17A—H17F109.5
C16—C18—H18A109.5C16A—C18A—H18D109.5
C16—C18—H18B109.5C16A—C18A—H18E109.5
H18A—C18—H18B109.5H18D—C18A—H18E109.5
C16—C18—H18C109.5C16A—C18A—H18F109.5
H18A—C18—H18C109.5H18D—C18A—H18F109.5
H18B—C18—H18C109.5H18E—C18A—H18F109.5
C21—C19—N4115.3 (7)N4A—C19A—C20A112.6 (14)
C21—C19—C20108.8 (5)N4A—C19A—C21A107.6 (16)
N4—C19—C20111.8 (7)C20A—C19A—C21A110.9 (10)
C21—C19—H19A106.8N4A—C19A—H19B108.5
N4—C19—H19A106.8C20A—C19A—H19B108.5
C20—C19—H19A106.8C21A—C19A—H19B108.5
C19—C20—H20A109.5C19A—C20A—H20D109.5
C19—C20—H20B109.5C19A—C20A—H20E109.5
H20A—C20—H20B109.5H20D—C20A—H20E109.5
C19—C20—H20C109.5C19A—C20A—H20F109.5
H20A—C20—H20C109.5H20D—C20A—H20F109.5
H20B—C20—H20C109.5H20E—C20A—H20F109.5
C19—C21—H21A109.5C19A—C21A—H21D109.5
C19—C21—H21B109.5C19A—C21A—H21E109.5
H21A—C21—H21B109.5H21D—C21A—H21E109.5
C19—C21—H21C109.5C19A—C21A—H21F109.5
H21A—C21—H21C109.5H21D—C21A—H21F109.5
H21B—C21—H21C109.5H21E—C21A—H21F109.5
C24—C22—N4112.0 (7)C23A—C22A—C24A105.5 (8)
C24—C22—C23108.3 (5)C23A—C22A—N4A111.8 (12)
N4—C22—C23109.1 (8)C24A—C22A—N4A112.0 (14)
C24—C22—H22A109.1C23A—C22A—H22B109.1
N4—C22—H22A109.1C24A—C22A—H22B109.1
C23—C22—H22A109.1N4A—C22A—H22B109.1
C22—C23—H23A109.5C22A—C23A—H23D109.5
C22—C23—H23B109.5C22A—C23A—H23E109.5
H23A—C23—H23B109.5H23D—C23A—H23E109.5
C22—C23—H23C109.5C22A—C23A—H23F109.5
H23A—C23—H23C109.5H23D—C23A—H23F109.5
H23B—C23—H23C109.5H23E—C23A—H23F109.5
C22—C24—H24A109.5C22A—C24A—H24D109.5
C22—C24—H24B109.5C22A—C24A—H24E109.5
H24A—C24—H24B109.5H24D—C24A—H24E109.5
C22—C24—H24C109.5C22A—C24A—H24F109.5
H24A—C24—H24C109.5H24D—C24A—H24F109.5
H24B—C24—H24C109.5H24E—C24A—H24F109.5
N1—P1—P2—N3132.8 (4)C1—N1—C4—C696.8 (7)
N1—P1—P2—N414.7 (5)P1—N1—C4—C6−63.7 (5)
N2—P1—P2—N3−112.2 (6)P1—N2—C7—C9116.3 (12)
N2—P1—P2—N4129.7 (6)P1—N2—C7—C8−118.7 (11)
C7—N2—P1—N162.6 (14)C10—N2—C7—C9−70.7 (10)
C10—N2—P1—N1−110.2 (9)C10—N2—C7—C854.2 (12)
C7—N2—P1—P2−50.6 (13)C7—N2—C10—C11−109.2 (10)
C10—N2—P1—P2136.6 (8)P1—N2—C10—C1165.0 (11)
C4—N1—P1—N2131.3 (4)C7—N2—C10—C12123.8 (9)
C1—N1—P1—N2−27.2 (7)P1—N2—C10—C12−62.0 (11)
C4—N1—P1—P2−127.5 (4)C16—N3—C13—C14132.0 (8)
C1—N1—P1—P274.0 (5)P2—N3—C13—C14−60.8 (9)
C22—N4—P2—N3130.9 (12)C16—N3—C13—C15−101.7 (9)
C19—N4—P2—N3−35.4 (16)P2—N3—C13—C1565.5 (9)
C22—N4—P2—P1−124.2 (12)C13—N3—C16—C17−73.1 (9)
C19—N4—P2—P169.5 (13)P2—N3—C16—C17121.1 (8)
C16—N3—P2—N465.3 (14)C13—N3—C16—C1853.2 (9)
C13—N3—P2—N4−99.9 (9)P2—N3—C16—C18−112.5 (10)
C16—N3—P2—P1−51.1 (10)C22—N4—C19—C2164.3 (13)
C13—N3—P2—P1143.7 (7)P2—N4—C19—C21−128.3 (11)
C4—N1—C1—C2−59.5 (7)C22—N4—C19—C20−60.7 (13)
P1—N1—C1—C299.9 (7)P2—N4—C19—C20106.8 (11)
C4—N1—C1—C363.8 (7)C19—N4—C22—C24−133.6 (10)
P1—N1—C1—C3−136.8 (6)P2—N4—C22—C2459.0 (15)
C1—N1—C4—C5−138.7 (4)C19—N4—C22—C23106.5 (11)
P1—N1—C4—C560.8 (5)P2—N4—C22—C23−60.9 (13)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: PV2196).

References

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