Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802007213/cf6161sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802007213/cf6161Isup2.hkl |
CCDC reference: 185763
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å
- R factor = 0.032
- wR factor = 0.106
- Data-to-parameter ratio = 13.3
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
1,2-Bis(diphenylphosphino)ethene was prepared from chlorodiphenylphosphine, by treatment with lithium, trimethylsilyl chloride and 1,2-dichloroethene in three stages. The ligand (88 mg, 0.22 mmol) was dissolved in ethanol (1 mmol) and Ni(ClO4)·6H2O (40 mg, 0.11 mmol) was added in acetonitrile, with stirring at room temperature. The filtered red solution was subjected to vapour diffussion by diethyl ether for several weeks, yielding orange crystals suitable for X-ray diffraction analysis.
All H atoms were placed in geometrically calculated positions and constrained with C—H = 0.96 Å and Uiso(H) = 1.2Ueq(C).
Data collection: CAD-4-PC (Enraf-Nonius, 1989); cell refinement: CAD-4-PC; data reduction: TEXSAN (Molecular Structure Corporation, 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
Fig. 1. The cation of the title compound, with 30% probability displacement ellipsoids. | |
Fig. 2. The crystal packing, viewed down the c axis. |
[Ni(C26H22P2)2](ClO4)2 | F(000) = 1084 |
Mr = 1050.34 | Dx = 1.511 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 25 reflections |
a = 10.845 (1) Å | θ = 9.2–13.9° |
b = 16.198 (1) Å | µ = 0.73 mm−1 |
c = 13.198 (1) Å | T = 293 K |
β = 95.26 (1)° | Block, orange |
V = 2308.7 (3) Å3 | 0.30 × 0.20 × 0.20 mm |
Z = 2 |
Enraf-Nonius CAD-4 diffractometer | 3195 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.056 |
Graphite monochromator | θmax = 25.0°, θmin = 2.0° |
ω/2θ scans | h = −12→12 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→19 |
Tmin = 0.839, Tmax = 0.864 | l = 0→15 |
4029 measured reflections | 5 standard reflections every 100 reflections |
4029 independent reflections | intensity decay: none |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.106 | H-atom parameters constrained |
S = 0.91 | w = 1/[σ2(Fo2) + (0.03P)2 + 0.65P] where P = (Fo2 + 2Fc2)/3 |
4029 reflections | (Δ/σ)max = 0.001 |
304 parameters | Δρmax = 0.33 e Å−3 |
0 restraints | Δρmin = −0.43 e Å−3 |
[Ni(C26H22P2)2](ClO4)2 | V = 2308.7 (3) Å3 |
Mr = 1050.34 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.845 (1) Å | µ = 0.73 mm−1 |
b = 16.198 (1) Å | T = 293 K |
c = 13.198 (1) Å | 0.30 × 0.20 × 0.20 mm |
β = 95.26 (1)° |
Enraf-Nonius CAD-4 diffractometer | 3195 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.056 |
Tmin = 0.839, Tmax = 0.864 | 5 standard reflections every 100 reflections |
4029 measured reflections | intensity decay: none |
4029 independent reflections |
R[F2 > 2σ(F2)] = 0.032 | 0 restraints |
wR(F2) = 0.106 | H-atom parameters constrained |
S = 0.91 | Δρmax = 0.33 e Å−3 |
4029 reflections | Δρmin = −0.43 e Å−3 |
304 parameters |
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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 0.7755 (0.0187) x - 15.3579 (0.0091) y + 4.1569 (0.0211) z = 1.9792 (0.0164) * 0.0169 (0.0024) C41 * -0.0200 (0.0028) C42 * 0.0013 (0.0034) C43 * 0.0209 (0.0036) C44 * -0.0249 (0.0034) C45 * 0.0058 (0.0029) C46 Rms deviation of fitted atoms = 0.0172 8.6617 (0.0098) x + 9.6128 (0.0200) y + 0.3423 (0.0229) z = 2.0423 (0.0142) Angle to previous plane (with approximate e.s.d.) = 53.92 (0.13) * -0.0083 (0.0022) C31 * -0.0020 (0.0029) C32 * 0.0136 (0.0030) C33 * -0.0150 (0.0028) C34 * 0.0048 (0.0027) C35 * 0.0069 (0.0023) C36 Rms deviation of fitted atoms = 0.0096 8.2028 (0.0121) x - 2.9101 (0.0245) y + 7.3513 (0.0184) z = 3.1605 (0.0128) Angle to previous plane (with approximate e.s.d.) = 55.94 (0.12) * -0.0084 (0.0023) C21 * 0.0226 (0.0025) C22 * -0.0176 (0.0030) C23 * -0.0019 (0.0031) C24 * 0.0153 (0.0030) C25 * -0.0101 (0.0027) C26 Rms deviation of fitted atoms = 0.0143 7.2749 (0.0144) x + 11.7191 (0.0203) y - 2.9546 (0.0232) z = 0.6019 (0.0082) Angle to previous plane (with approximate e.s.d.) = 74.05 (0.12) * -0.0165 (0.0027) C11 * 0.0037 (0.0026) C12 * 0.0135 (0.0029) C13 * -0.0171 (0.0032) C14 * 0.0033 (0.0035) C15 * 0.0132 (0.0033) C16 Rms deviation of fitted atoms = 0.0126 - 8.7419 (0.0039) x - 9.3212 (0.0075) y + 2.7912 (0.0010) z = 0.2791 (0.0001) Angle to previous plane (with approximate e.s.d.) = 11.60 (0.18) * -0.5297 (0.0003) P1 * -0.5696 (0.0003) P2 * 1.1165 (0.0004) Ni * -0.0285 (0.0003) P1_$1 * 0.0114 (0.0002) P2_$1 Rms deviation of fitted atoms = 0.6087 |
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. |
x | y | z | Uiso*/Ueq | ||
Ni | 0.0000 | 0.0000 | 0.5000 | 0.02783 (15) | |
P1 | 0.03577 (7) | 0.12371 (5) | 0.43539 (7) | 0.0517 (2) | |
P2 | 0.20327 (7) | 0.00574 (5) | 0.55170 (7) | 0.0529 (2) | |
C11 | −0.0311 (3) | 0.1488 (2) | 0.3155 (3) | 0.0626 (7) | |
C12 | −0.1252 (3) | 0.2047 (2) | 0.2989 (2) | 0.0548 (7) | |
H12A | −0.1466 | 0.2369 | 0.3558 | 0.080* | |
C13 | −0.1830 (4) | 0.2181 (2) | 0.2064 (3) | 0.0700 (9) | |
H13A | −0.2395 | 0.2636 | 0.1961 | 0.080* | |
C14 | −0.1479 (5) | 0.1753 (3) | 0.1330 (3) | 0.0825 (11) | |
H14A | −0.2011 | 0.1735 | 0.0707 | 0.080* | |
C16 | 0.0085 (5) | 0.1068 (2) | 0.2365 (3) | 0.0889 (13) | |
H16A | 0.0811 | 0.0727 | 0.2429 | 0.080* | |
C21 | 0.0017 (3) | 0.21010 (18) | 0.5101 (2) | 0.0516 (6) | |
C22 | −0.0696 (3) | 0.2012 (2) | 0.5903 (3) | 0.0648 (8) | |
H22A | −0.0958 | 0.1468 | 0.6076 | 0.080* | |
C23 | −0.0975 (4) | 0.2652 (3) | 0.6413 (3) | 0.0827 (10) | |
H23A | −0.1538 | 0.2581 | 0.6927 | 0.080* | |
C24 | −0.0539 (5) | 0.3428 (3) | 0.6255 (3) | 0.0901 (12) | |
H24A | −0.0758 | 0.3897 | 0.6645 | 0.080* | |
C25 | 0.0208 (5) | 0.3528 (2) | 0.5485 (3) | 0.0910 (12) | |
H25A | 0.0594 | 0.4051 | 0.5382 | 0.080* | |
C26 | 0.0448 (4) | 0.2875 (2) | 0.4924 (3) | 0.0744 (10) | |
H26A | 0.0869 | 0.2959 | 0.4324 | 0.080* | |
C31 | 0.3042 (2) | −0.0818 (2) | 0.5411 (2) | 0.0489 (6) | |
C32 | 0.3373 (4) | −0.1077 (3) | 0.4522 (3) | 0.0802 (11) | |
H32A | 0.3000 | −0.0800 | 0.3928 | 0.080* | |
C34 | 0.4558 (4) | −0.2185 (3) | 0.5240 (3) | 0.0756 (9) | |
H34A | 0.5105 | −0.2642 | 0.5165 | 0.080* | |
C35 | 0.4264 (4) | −0.1930 (2) | 0.6098 (3) | 0.0699 (9) | |
H35A | 0.4534 | −0.2248 | 0.6691 | 0.080* | |
C36 | 0.3524 (3) | −0.12651 (17) | 0.6227 (2) | 0.0481 (6) | |
H36A | 0.3349 | −0.1104 | 0.6899 | 0.080* | |
C41 | 0.2284 (3) | 0.04100 (18) | 0.6743 (2) | 0.0536 (6) | |
C42 | 0.3471 (3) | 0.0498 (2) | 0.7199 (3) | 0.0698 (9) | |
H42A | 0.4165 | 0.0398 | 0.6814 | 0.080* | |
C43 | 0.3644 (4) | 0.0742 (3) | 0.8185 (4) | 0.0876 (12) | |
H43A | 0.4459 | 0.0781 | 0.8533 | 0.080* | |
C44 | 0.2653 (4) | 0.0915 (3) | 0.8686 (4) | 0.0913 (13) | |
H44A | 0.2751 | 0.1050 | 0.9397 | 0.080* | |
C45 | 0.1476 (4) | 0.0869 (3) | 0.8187 (4) | 0.0835 (11) | |
H45A | 0.0808 | 0.1065 | 0.8552 | 0.080* | |
C46 | 0.1280 (3) | 0.0608 (2) | 0.7261 (3) | 0.0670 (8) | |
H46A | 0.0462 | 0.0521 | 0.6937 | 0.080* | |
Cl | 0.76535 (10) | 0.08822 (7) | 0.83109 (7) | 0.0756 (3) | |
O1 | 0.7351 (9) | 0.1666 (4) | 0.8218 (5) | 0.247 (4) | |
O2 | 0.6706 (7) | 0.0509 (5) | 0.8487 (6) | 0.222 (3) | |
O3 | 0.8277 (6) | 0.0642 (4) | 0.7527 (4) | 0.187 (2) | |
O4 | 0.8352 (8) | 0.0572 (6) | 0.9128 (4) | 0.235 (3) | |
C33 | 0.4117 (4) | −0.1728 (4) | 0.4433 (3) | 0.0872 (11) | |
H33A | 0.4339 | −0.1894 | 0.3776 | 0.080* | |
C15 | −0.0543 (6) | 0.1213 (3) | 0.1428 (3) | 0.1006 (16) | |
H15A | −0.0263 | 0.0950 | 0.0839 | 0.080* | |
C1 | 0.2030 (3) | 0.1316 (3) | 0.4225 (4) | 0.0854 (13) | |
H1A | 0.2353 | 0.1691 | 0.3752 | 0.080* | |
C2 | 0.2741 (4) | 0.0861 (3) | 0.4816 (4) | 0.0959 (15) | |
H2A | 0.3624 | 0.0925 | 0.4869 | 0.080* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni | 0.0327 (3) | 0.0270 (3) | 0.0234 (2) | −0.00064 (13) | 0.00114 (18) | 0.00066 (13) |
P1 | 0.0394 (4) | 0.0417 (4) | 0.0749 (5) | 0.0012 (3) | 0.0095 (4) | 0.0254 (4) |
P2 | 0.0356 (4) | 0.0636 (5) | 0.0574 (5) | −0.0090 (3) | −0.0069 (3) | 0.0296 (4) |
C11 | 0.0597 (17) | 0.0582 (19) | 0.0720 (15) | 0.0056 (14) | 0.0172 (14) | 0.0246 (14) |
C12 | 0.0562 (17) | 0.0597 (19) | 0.0493 (14) | 0.0057 (13) | 0.0084 (13) | 0.0111 (13) |
C13 | 0.080 (2) | 0.068 (2) | 0.0611 (17) | 0.0027 (17) | 0.0045 (16) | 0.0132 (16) |
C14 | 0.117 (3) | 0.074 (3) | 0.0549 (17) | −0.0213 (19) | 0.0006 (19) | 0.0068 (16) |
C16 | 0.122 (3) | 0.066 (2) | 0.0870 (19) | 0.037 (2) | 0.053 (2) | 0.024 (2) |
C21 | 0.0505 (16) | 0.0306 (13) | 0.0689 (16) | −0.0037 (10) | −0.0197 (12) | 0.0199 (10) |
C22 | 0.065 (2) | 0.0527 (16) | 0.075 (2) | −0.0027 (15) | −0.0084 (14) | 0.0098 (14) |
C23 | 0.091 (3) | 0.080 (2) | 0.075 (2) | −0.001 (2) | −0.0045 (19) | 0.0022 (18) |
C24 | 0.116 (3) | 0.066 (2) | 0.080 (2) | −0.009 (2) | −0.0355 (19) | −0.0189 (19) |
C25 | 0.132 (4) | 0.0461 (18) | 0.087 (3) | −0.015 (2) | −0.033 (2) | 0.0144 (16) |
C26 | 0.096 (3) | 0.0480 (16) | 0.075 (2) | −0.0243 (18) | −0.0176 (17) | 0.0184 (14) |
C31 | 0.0280 (11) | 0.0775 (17) | 0.0407 (12) | −0.0078 (11) | −0.0004 (10) | 0.0128 (11) |
C32 | 0.0555 (19) | 0.143 (3) | 0.0412 (14) | −0.0018 (19) | −0.0010 (14) | 0.0051 (18) |
C34 | 0.055 (2) | 0.085 (3) | 0.088 (2) | −0.0041 (17) | 0.0127 (17) | −0.0165 (19) |
C35 | 0.073 (2) | 0.069 (2) | 0.0681 (18) | 0.0105 (16) | 0.0099 (17) | 0.0032 (17) |
C36 | 0.0566 (17) | 0.0425 (14) | 0.0440 (13) | −0.0058 (11) | −0.0023 (12) | 0.0058 (11) |
C41 | 0.0483 (14) | 0.0400 (14) | 0.0687 (12) | −0.0061 (11) | −0.0141 (11) | 0.0128 (11) |
C42 | 0.0480 (15) | 0.0561 (18) | 0.101 (2) | −0.0084 (15) | −0.0154 (16) | −0.0110 (18) |
C43 | 0.065 (2) | 0.076 (2) | 0.115 (3) | −0.008 (2) | −0.0263 (19) | −0.036 (2) |
C44 | 0.086 (2) | 0.098 (3) | 0.085 (3) | −0.012 (2) | −0.0181 (18) | −0.028 (2) |
C45 | 0.070 (2) | 0.091 (3) | 0.089 (2) | −0.009 (2) | 0.0048 (18) | −0.019 (2) |
C46 | 0.0511 (16) | 0.066 (2) | 0.0813 (19) | −0.0173 (15) | −0.0077 (14) | 0.0014 (17) |
Cl | 0.0793 (6) | 0.0904 (7) | 0.0606 (5) | 0.0006 (5) | 0.0257 (5) | −0.0144 (4) |
O1 | 0.434 (11) | 0.128 (3) | 0.207 (6) | 0.077 (4) | 0.182 (7) | 0.021 (4) |
O2 | 0.181 (4) | 0.216 (6) | 0.284 (8) | −0.042 (5) | 0.104 (4) | −0.019 (6) |
O3 | 0.235 (6) | 0.212 (5) | 0.126 (3) | 0.083 (4) | 0.088 (4) | −0.005 (3) |
O4 | 0.260 (6) | 0.330 (9) | 0.114 (3) | 0.101 (7) | 0.014 (4) | 0.010 (5) |
C33 | 0.063 (2) | 0.139 (4) | 0.0630 (19) | −0.013 (2) | 0.0220 (17) | 0.001 (2) |
C15 | 0.175 (5) | 0.066 (3) | 0.0690 (18) | 0.017 (3) | 0.055 (2) | 0.005 (2) |
C1 | 0.0373 (15) | 0.081 (2) | 0.131 (3) | 0.0041 (15) | 0.0244 (17) | 0.063 (2) |
C2 | 0.0382 (16) | 0.134 (3) | 0.106 (3) | −0.0185 (19) | 0.0065 (19) | 0.069 (3) |
Ni—P1i | 2.2258 (7) | C31—C32 | 1.327 (5) |
Ni—P1 | 2.2258 (7) | C31—C36 | 1.361 (4) |
Ni—P2 | 2.2490 (8) | C32—C33 | 1.339 (7) |
Ni—P2i | 2.2490 (8) | C32—H32A | 0.960 |
P1—C11 | 1.728 (4) | C34—C35 | 1.272 (5) |
P1—C21 | 1.770 (4) | C34—C33 | 1.347 (6) |
P1—C1 | 1.841 (4) | C34—H34A | 0.960 |
P2—C41 | 1.714 (3) | C35—C36 | 1.364 (5) |
P2—C31 | 1.805 (3) | C35—H35A | 0.960 |
P2—C2 | 1.809 (4) | C36—H36A | 0.960 |
C11—C16 | 1.348 (5) | C41—C42 | 1.378 (4) |
C11—C12 | 1.367 (5) | C41—C46 | 1.376 (5) |
C12—C13 | 1.338 (5) | C42—C43 | 1.356 (6) |
C12—H12A | 0.960 | C42—H42A | 0.960 |
C13—C14 | 1.277 (6) | C43—C44 | 1.343 (7) |
C13—H13A | 0.960 | C43—H43A | 0.960 |
C14—C15 | 1.337 (7) | C44—C45 | 1.383 (6) |
C14—H14A | 0.960 | C44—H44A | 0.960 |
C16—C15 | 1.376 (7) | C45—C46 | 1.292 (6) |
C16—H16A | 0.960 | C45—H45A | 0.960 |
C21—C26 | 1.365 (4) | C46—H46A | 0.960 |
C21—C22 | 1.374 (5) | Cl—O2 | 1.232 (6) |
C22—C23 | 1.287 (6) | Cl—O1 | 1.314 (6) |
C22—H22A | 0.960 | Cl—O4 | 1.357 (7) |
C23—C24 | 1.365 (6) | Cl—O3 | 1.344 (4) |
C23—H23A | 0.960 | C33—H33A | 0.960 |
C24—C25 | 1.366 (7) | C15—H15A | 0.960 |
C24—H24A | 0.960 | C1—C2 | 1.279 (5) |
C25—C26 | 1.331 (6) | C1—H1A | 0.960 |
C25—H25A | 0.960 | C2—H2A | 0.960 |
C26—H26A | 0.960 | ||
P1i—Ni—P1 | 180.00 | C32—C31—C36 | 114.6 (3) |
P1i—Ni—P2 | 96.97 (3) | C32—C31—P2 | 122.2 (3) |
P1—Ni—P2 | 83.03 (3) | C36—C31—P2 | 123.3 (2) |
P1i—Ni—P2i | 83.03 (3) | C31—C32—C33 | 122.7 (4) |
P1—Ni—P2i | 96.97 (3) | C31—C32—H32A | 116.6 |
P2—Ni—P2i | 180.0 | C33—C32—H32A | 120.6 |
C11—P1—C21 | 103.44 (15) | C35—C34—C33 | 115.2 (4) |
C11—P1—C1 | 103.50 (18) | C35—C34—H34A | 123.3 |
C21—P1—C1 | 104.74 (19) | C33—C34—H34A | 121.3 |
C11—P1—Ni | 119.31 (13) | C34—C35—C36 | 124.4 (4) |
C21—P1—Ni | 116.45 (10) | C34—C35—H35A | 118.0 |
C1—P1—Ni | 107.80 (12) | C36—C35—H35A | 117.4 |
C41—P2—C31 | 106.85 (14) | C31—C36—C35 | 120.6 (3) |
C41—P2—C2 | 101.8 (2) | C31—C36—H36A | 119.5 |
C31—P2—C2 | 103.7 (2) | C35—C36—H36A | 119.9 |
C41—P2—Ni | 111.51 (12) | C42—C41—C46 | 120.5 (3) |
C31—P2—Ni | 121.93 (10) | C42—C41—P2 | 120.6 (3) |
C2—P2—Ni | 108.96 (13) | C46—C41—P2 | 118.9 (2) |
C16—C11—C12 | 119.8 (4) | C43—C42—C41 | 119.5 (4) |
C16—C11—P1 | 116.9 (3) | C43—C42—H42A | 120.7 |
C12—C11—P1 | 123.2 (3) | C41—C42—H42A | 119.8 |
C13—C12—C11 | 122.3 (4) | C44—C43—C42 | 119.1 (4) |
C13—C12—H12A | 120.0 | C44—C43—H43A | 119.6 |
C11—C12—H12A | 117.6 | C42—C43—H43A | 121.3 |
C14—C13—C12 | 117.2 (4) | C43—C44—C45 | 120.0 (4) |
C14—C13—H13A | 122.7 | C43—C44—H44A | 120.5 |
C12—C13—H13A | 119.5 | C45—C44—H44A | 119.5 |
C13—C14—C15 | 123.9 (4) | C46—C45—C44 | 122.2 (5) |
C13—C14—H14A | 117.9 | C46—C45—H45A | 121.1 |
C15—C14—H14A | 117.1 | C44—C45—H45A | 116.7 |
C11—C16—C15 | 116.3 (4) | C45—C46—C41 | 118.5 (4) |
C11—C16—H16A | 122.7 | C45—C46—H46A | 122.3 |
C15—C16—H16A | 120.7 | C41—C46—H46A | 119.0 |
C26—C21—C22 | 117.0 (4) | O2—Cl—O1 | 106.6 (5) |
C26—C21—P1 | 122.5 (3) | O2—Cl—O4 | 94.7 (6) |
C22—C21—P1 | 120.5 (2) | O1—Cl—O4 | 123.3 (5) |
C23—C22—C21 | 119.6 (4) | O2—Cl—O3 | 119.4 (5) |
C23—C22—H22A | 121.7 | O1—Cl—O3 | 110.3 (4) |
C21—C22—H22A | 118.6 | O4—Cl—O3 | 102.8 (4) |
C22—C23—C24 | 124.1 (5) | C32—C33—C34 | 122.4 (4) |
C22—C23—H23A | 117.9 | C32—C33—H33A | 120.2 |
C24—C23—H23A | 118.0 | C34—C33—H33A | 117.4 |
C25—C24—C23 | 117.4 (4) | C14—C15—C16 | 120.5 (4) |
C25—C24—H24A | 119.8 | C14—C15—H15A | 120.3 |
C23—C24—H24A | 122.8 | C16—C15—H15A | 119.0 |
C26—C25—C24 | 118.6 (4) | C2—C1—P1 | 116.6 (3) |
C26—C25—H25A | 120.8 | C2—C1—H1A | 121.7 |
C24—C25—H25A | 120.4 | P1—C1—H1A | 121.7 |
C25—C26—C21 | 123.2 (4) | C1—C2—P2 | 117.8 (3) |
C25—C26—H26A | 118.6 | C1—C2—H2A | 121.6 |
C21—C26—H26A | 117.9 | P2—C2—H2A | 120.6 |
Symmetry code: (i) −x, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Ni(C26H22P2)2](ClO4)2 |
Mr | 1050.34 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 10.845 (1), 16.198 (1), 13.198 (1) |
β (°) | 95.26 (1) |
V (Å3) | 2308.7 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.73 |
Crystal size (mm) | 0.30 × 0.20 × 0.20 |
Data collection | |
Diffractometer | Enraf-Nonius CAD-4 diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.839, 0.864 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4029, 4029, 3195 |
Rint | 0.056 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.032, 0.106, 0.91 |
No. of reflections | 4029 |
No. of parameters | 304 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.33, −0.43 |
Computer programs: CAD-4-PC (Enraf-Nonius, 1989), CAD-4-PC, TEXSAN (Molecular Structure Corporation, 1989), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997), SHELXL97.
Ni—P1 | 2.2258 (7) | P2—C2 | 1.809 (4) |
Ni—P2 | 2.2490 (8) | C1—C2 | 1.279 (5) |
P1—C1 | 1.841 (4) | ||
P1i—Ni—P2 | 96.97 (3) | C2—C1—P1 | 116.6 (3) |
C1—P1—Ni | 107.80 (12) | C1—C2—P2 | 117.8 (3) |
C2—P2—Ni | 108.96 (13) |
Symmetry code: (i) −x, −y, −z+1. |
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In recent years, much attention has been given to transition metal phosphine complexes for their antitumor activities and catalysis. We have synthesized the title compound, (I), and determined its crystal structure. The Ni atom lies on an inversion centre and is square-planar coordinated by four P atoms from two bidentate ligands. The average Ni—P bond length is 2.2374 (7) Å, with individual values of 2.2258 (7) and 2.2490 (8) Å. The connection of two phosphine groups by an ethene bridge is unusual, most diphosphines having saturated links composed of one or more methylene groups (Li et al., 2000).
In the title compound, (I) (Fig. 1), the phenyl groups lie approximately perpendicular to the metal coordination plane, with dihedral angles ranging from 76.0 (2) to 88.7 (2)°. The nickel centre is relatively exposed, and this may be the reason for the anti-tumor and catalytic activity of the complex.
The crystal packing is shown in Fig. 2.