Literature DB >> 25878844

Crystal structure of bis-[1,3-bis-(di-phenyl-phosphan-yl)propane-κ(2) P,P']platinum(II) dichloride chloro-form penta-solvate.

Bradley G Anderson1, Sarah A Hoyte1, John L Spencer1.   

Abstract

In the title compound, [Pt{Ph2P(CH2)3PPh2}2]Cl2·5CHCl3, the Pt(II) cations, located on a centre of inversion, is coordinated by two chelating diphosphane ligands in a geometry which is close to square-planar. The chelate rings adopt a chair conformation. The Pt(II) cations are arranged in layers separated by Cl(-) anions as well as CHCl3 solvent mol-ecules. While this complex has been reported previously [Anderson et al. (1983 ▶). Inorg. Chim. Acta, 76, L251-L252], this is the first time a structure has been determined.

Entities:  

Keywords:  1,3-bis­(di­phenyl­phosphan­yl)propane; crystal structure; platinum(II) complex

Year:  2015        PMID: 25878844      PMCID: PMC4384563          DOI: 10.1107/S205698901500136X

Source DB:  PubMed          Journal:  Acta Crystallogr E Crystallogr Commun


Related literature

For structures of related group 10 M 2+ bis-diphosphane complexes, see: Pahor & Bruno (1977 ▸); Engelhardt et al. (1984 ▸); Ferguson et al. (1993 ▸); Berning et al. (1999 ▸); Raebiger et al. (2004 ▸); Fischer (2006 ▸). The corresponding Pt0 complex [Pt(dppp)2] [dppp is 1,3-bis­(di­phenyl­phosphan­yl)propane] has been reported by Asker et al. (1990 ▸). For a previous report of the title compound, see: Anderson et al. (1983 ▸).

Experimental

Crystal data

[Pt(C27H26P2)2]Cl2·5CHCl3 M = 1687.67 Orthorhombic, a = 26.2042 (9) Å b = 15.3120 (5) Å c = 16.7930 (5) Å V = 6738.0 (4) Å3 Z = 4 Mo Kα radiation μ = 2.89 mm−1 T = 160 K 0.60 × 0.38 × 0.28 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2007 ▸) T min = 0.562, T max = 0.746 179974 measured reflections 10325 independent reflections 7580 reflections with I > 2σ(I) R int = 0.063

Refinement

R[F 2 > 2σ(F 2)] = 0.037 wR(F 2) = 0.073 S = 1.20 10325 reflections 385 parameters H-atom parameters constrained Δρmax = 0.73 e Å−3 Δρmin = −0.97 e Å−3

Data collection: APEX2 (Bruker, 2007 ▸); cell refinement: SAINT (Bruker, 2007 ▸); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▸); program(s) used to refine structure: SHELXL97 (Sheldrick, 2015 ▸); molecular graphics: Mercury (Macrae et al., 2008 ▸); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablock(s) I. DOI: 10.1107/S205698901500136X/gg2144sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S205698901500136X/gg2144Isup2.hkl Click here for additional data file. ORTEP 2 2 3 2 2 2 . DOI: 10.1107/S205698901500136X/gg2144fig1.tif ORTEP diagram of [Pt(Ph2P(C2H3)PPh2)2]Cl2 showing 50% probability ellipsoids. H atoms have been omitted for clarity. CCDC reference: 1044833 Additional supporting information: crystallographic information; 3D view; checkCIF report
[Pt(C27H26P2)2]Cl2·5CHCl3F(000) = 3352.00
Mr = 1687.67Dx = 1.664 Mg m3
Orthorhombic, PccnMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ab 2acCell parameters from 9982 reflections
a = 26.2042 (9) Åθ = 2.4–30.5°
b = 15.3120 (5) ŵ = 2.89 mm1
c = 16.7930 (5) ÅT = 160 K
V = 6738.0 (4) Å3Block, colourless
Z = 40.6 × 0.38 × 0.28 mm
Bruker APEXII CCD diffractometer10325 independent reflections
Radiation source: fine-focus sealed tube7580 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.063
φ and ω scansθmax = 30.6°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Bruker, 2007)h = −37→37
Tmin = 0.562, Tmax = 0.746k = −21→21
179974 measured reflectionsl = −23→24
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.073H-atom parameters constrained
S = 1.20w = 1/[σ2(Fo2) + (0.P)2 + 21.821P] where P = (Fo2 + 2Fc2)/3
10325 reflections(Δ/σ)max = 0.001
385 parametersΔρmax = 0.73 e Å3
0 restraintsΔρmin = −0.97 e Å3
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.
xyzUiso*/UeqOcc. (<1)
Pt10.50000.00000.00000.01283 (4)
P20.49876 (3)0.10087 (5)0.10661 (4)0.01623 (14)
P10.48568 (3)−0.11136 (5)0.09623 (4)0.01524 (15)
C40.41837 (12)−0.1208 (2)0.11952 (18)0.0178 (6)
C30.52924 (13)0.0645 (2)0.19883 (18)0.0210 (6)
H3A0.56480.05190.18750.025*
H3B0.52840.11230.23670.025*
C180.53826 (15)0.3596 (2)0.1019 (2)0.0278 (8)
H180.52190.41330.10610.033*
C10.51746 (13)−0.0980 (2)0.19268 (17)0.0194 (6)
H1A0.5082−0.14720.22610.023*
H1B0.5540−0.10090.18410.023*
C210.58744 (13)0.1990 (2)0.0910 (2)0.0234 (7)
H210.60400.14530.08860.028*
C20.50582 (13)−0.0150 (2)0.23790 (17)0.0211 (7)
H2A0.5188−0.02020.29180.025*
H2B0.4691−0.00740.24100.025*
C90.40155 (13)−0.1654 (2)0.18772 (19)0.0219 (7)
H90.4251−0.18790.22370.026*
C220.43463 (13)0.1321 (2)0.13539 (19)0.0203 (6)
C140.49389 (16)−0.3787 (2)0.0796 (2)0.0299 (8)
H140.4719−0.42620.08330.036*
C50.38263 (13)−0.0870 (2)0.0673 (2)0.0239 (7)
H50.3934−0.05680.02220.029*
C80.34994 (14)−0.1758 (3)0.2012 (2)0.0294 (8)
H80.3389−0.20570.24610.035*
C160.53416 (12)0.2026 (2)0.09712 (18)0.0183 (6)
C190.59096 (16)0.3563 (3)0.0944 (2)0.0316 (8)
H190.60990.40770.09320.038*
C170.50980 (13)0.2833 (2)0.10331 (18)0.0217 (7)
H170.47450.28590.10840.026*
C110.56005 (14)−0.2376 (2)0.0705 (2)0.0251 (7)
H110.5824−0.19050.06790.030*
C100.50772 (13)−0.22317 (19)0.07887 (17)0.0189 (6)
C60.33060 (14)−0.0978 (3)0.0817 (2)0.0352 (9)
H60.3068−0.07520.04630.042*
C120.57854 (16)−0.3223 (3)0.0660 (2)0.0326 (9)
H120.6134−0.33200.05980.039*
C150.47444 (14)−0.2942 (2)0.08337 (18)0.0214 (7)
H150.4395−0.28520.08880.026*
C230.39470 (13)0.1199 (2)0.0827 (2)0.0236 (7)
H230.40080.09380.03360.028*
C200.61522 (15)0.2762 (2)0.0886 (2)0.0291 (8)
H200.65050.27410.08300.035*
C70.31462 (15)−0.1420 (3)0.1484 (2)0.0352 (9)
H70.2799−0.14920.15810.042*
C130.54565 (17)−0.3923 (3)0.0706 (2)0.0350 (9)
H130.5583−0.44890.06760.042*
C260.37622 (16)0.1975 (3)0.2287 (3)0.0365 (9)
H260.36980.22350.27780.044*
C240.34563 (15)0.1462 (3)0.1022 (3)0.0343 (9)
H240.31890.13770.06650.041*
C270.42495 (15)0.1714 (3)0.2095 (2)0.0288 (8)
H270.45150.17980.24550.035*
C250.33674 (16)0.1853 (3)0.1753 (3)0.0414 (10)
H250.30390.20340.18850.050*
Cl10.35882 (4)0.04388 (8)−0.11105 (5)0.0380 (2)
Cl3B0.31059 (4)0.01417 (7)0.32358 (6)0.0371 (2)
Cl2A0.21666 (4)0.05178 (8)0.17673 (6)0.0434 (3)
Cl2B0.24294 (5)−0.13417 (8)0.34282 (7)0.0475 (3)
Cl3A0.14625 (5)−0.09321 (7)0.16878 (7)0.0430 (2)
Cl1A0.11366 (4)0.07947 (8)0.12128 (7)0.0447 (3)
Cl1B0.29044 (4)−0.05640 (10)0.48005 (6)0.0523 (3)
C1B0.26446 (14)−0.0355 (3)0.3849 (2)0.0328 (8)
H1BA0.23540.00420.39070.039*
C1A0.15290 (14)0.0195 (3)0.1870 (2)0.0304 (8)
H1AA0.14200.03150.24170.036*
C1C0.2657 (3)0.2740 (5)0.4313 (4)0.0282 (15)0.5
H1C0.29540.31150.42180.034*0.5
Cl3C0.23595 (11)0.2360 (3)0.34548 (14)0.0622 (9)0.5
Cl1C0.2171 (5)0.3222 (11)0.4886 (6)0.076 (3)0.5
Cl2C0.2802 (3)0.1693 (9)0.4893 (3)0.0494 (17)0.5
U11U22U33U12U13U23
Pt10.01516 (6)0.01052 (6)0.01280 (6)0.00000 (7)0.00067 (6)0.00078 (6)
P20.0207 (4)0.0126 (3)0.0154 (3)−0.0020 (3)0.0032 (3)−0.0003 (3)
P10.0192 (4)0.0124 (3)0.0141 (3)0.0011 (3)0.0022 (3)0.0021 (3)
C40.0193 (15)0.0149 (15)0.0190 (14)−0.0017 (12)0.0029 (11)−0.0026 (11)
C30.0254 (17)0.0203 (16)0.0174 (14)−0.0028 (13)−0.0029 (12)0.0006 (12)
C180.044 (2)0.0149 (16)0.0248 (17)−0.0045 (15)0.0073 (15)−0.0037 (13)
C10.0232 (15)0.0188 (15)0.0163 (13)0.0000 (13)−0.0023 (11)0.0029 (11)
C210.0261 (17)0.0215 (17)0.0227 (15)−0.0029 (14)−0.0008 (13)0.0006 (13)
C20.0278 (18)0.0213 (17)0.0141 (12)−0.0034 (13)−0.0035 (12)0.0021 (10)
C90.0237 (17)0.0212 (16)0.0208 (15)0.0015 (13)0.0028 (12)0.0020 (12)
C220.0258 (17)0.0141 (15)0.0211 (15)−0.0009 (13)0.0056 (12)0.0026 (12)
C140.049 (2)0.0157 (15)0.0253 (16)−0.0002 (16)0.0086 (16)0.0042 (12)
C50.0250 (17)0.0251 (18)0.0216 (15)−0.0006 (14)−0.0015 (13)0.0039 (13)
C80.0276 (19)0.033 (2)0.0280 (17)−0.0057 (16)0.0099 (14)−0.0017 (15)
C160.0240 (16)0.0164 (15)0.0146 (13)−0.0049 (12)0.0009 (11)−0.0003 (11)
C190.043 (2)0.0238 (18)0.0276 (17)−0.0149 (17)0.0017 (16)−0.0028 (15)
C170.0293 (19)0.0170 (15)0.0188 (14)0.0002 (13)0.0070 (12)0.0005 (11)
C110.0303 (19)0.0194 (17)0.0255 (16)0.0025 (14)0.0090 (14)0.0037 (13)
C100.0283 (19)0.0106 (13)0.0179 (13)0.0016 (12)0.0056 (12)0.0030 (10)
C60.0229 (18)0.046 (2)0.036 (2)0.0016 (17)−0.0060 (15)0.0019 (18)
C120.034 (2)0.0257 (19)0.038 (2)0.0122 (16)0.0134 (16)0.0076 (16)
C150.0292 (18)0.0194 (16)0.0156 (14)0.0002 (13)0.0032 (12)0.0016 (12)
C230.0254 (17)0.0175 (16)0.0280 (17)0.0003 (13)0.0041 (13)0.0015 (13)
C200.0284 (19)0.0282 (19)0.0307 (18)−0.0084 (15)−0.0007 (15)0.0007 (15)
C70.0206 (18)0.043 (2)0.042 (2)−0.0021 (17)0.0045 (16)−0.0016 (18)
C130.053 (3)0.0189 (18)0.0335 (19)0.0140 (18)0.0129 (17)0.0048 (15)
C260.037 (2)0.033 (2)0.039 (2)0.0013 (18)0.0192 (18)−0.0097 (17)
C240.0241 (19)0.031 (2)0.047 (2)−0.0007 (16)0.0024 (17)0.0015 (18)
C270.031 (2)0.031 (2)0.0245 (16)−0.0018 (16)0.0088 (14)−0.0058 (14)
C250.027 (2)0.035 (2)0.063 (3)0.0041 (17)0.018 (2)−0.001 (2)
Cl10.0287 (5)0.0622 (7)0.0231 (4)−0.0202 (5)−0.0050 (3)0.0069 (4)
Cl3B0.0336 (5)0.0431 (6)0.0346 (5)0.0032 (4)0.0003 (4)0.0038 (4)
Cl2A0.0321 (5)0.0565 (7)0.0417 (5)−0.0104 (5)−0.0056 (4)0.0056 (5)
Cl2B0.0446 (6)0.0378 (6)0.0602 (7)−0.0017 (5)0.0086 (5)−0.0088 (5)
Cl3A0.0497 (6)0.0355 (6)0.0437 (5)−0.0053 (5)−0.0016 (5)0.0020 (4)
Cl1A0.0346 (5)0.0484 (7)0.0510 (6)0.0033 (5)−0.0021 (5)0.0146 (5)
Cl1B0.0340 (5)0.0915 (10)0.0314 (5)0.0023 (6)0.0049 (4)0.0052 (5)
C1B0.0246 (19)0.038 (2)0.0358 (19)0.0078 (16)0.0004 (15)−0.0033 (17)
C1A0.031 (2)0.038 (2)0.0219 (16)−0.0022 (16)0.0035 (14)0.0008 (14)
C1C0.024 (4)0.030 (4)0.030 (3)0.000 (3)−0.004 (3)−0.001 (3)
Cl3C0.071 (3)0.073 (3)0.0421 (11)0.0157 (19)−0.0230 (11)−0.0151 (14)
Cl1C0.079 (6)0.076 (5)0.074 (5)0.046 (4)0.006 (4)−0.009 (3)
Cl2C0.045 (3)0.076 (4)0.027 (2)0.041 (3)0.0020 (18)0.005 (2)
Pt1—P22.3648 (7)C5—C61.395 (5)
Pt1—P2i2.3648 (7)C8—C71.381 (6)
Pt1—P12.3790 (8)C16—C171.395 (4)
Pt1—P1i2.3790 (8)C19—C201.385 (5)
P2—C31.829 (3)C11—C101.396 (5)
P2—C221.813 (3)C11—C121.387 (5)
P2—C161.820 (3)C10—C151.396 (4)
P1—C41.812 (3)C6—C71.374 (6)
P1—C11.833 (3)C12—C131.377 (6)
P1—C101.830 (3)C23—C241.386 (5)
C4—C91.404 (4)C26—C271.376 (5)
C4—C51.384 (5)C26—C251.382 (6)
C3—C21.513 (4)C24—C251.386 (6)
C18—C191.388 (5)Cl3B—C1B1.761 (4)
C18—C171.387 (5)Cl2A—C1A1.751 (4)
C1—C21.512 (4)Cl2B—C1B1.760 (4)
C21—C161.401 (5)Cl3A—C1A1.761 (4)
C21—C201.390 (5)Cl1A—C1A1.766 (4)
C9—C81.380 (5)Cl1B—C1B1.765 (4)
C22—C231.382 (5)C1C—Cl3C1.739 (7)
C22—C271.405 (5)C1C—Cl1C1.759 (13)
C14—C151.391 (5)C1C—Cl2C1.914 (14)
C14—C131.381 (6)
P2—Pt1—P2i180.0C4—C5—C6120.5 (3)
P2i—Pt1—P192.77 (3)C9—C8—C7120.6 (3)
P2—Pt1—P187.23 (3)C21—C16—P2118.7 (3)
P2—Pt1—P1i92.77 (3)C17—C16—P2121.2 (2)
P2i—Pt1—P1i87.23 (3)C17—C16—C21119.8 (3)
P1i—Pt1—P1180.0C20—C19—C18119.7 (3)
C3—P2—Pt1115.85 (11)C18—C17—C16119.9 (3)
C22—P2—Pt1112.76 (11)C12—C11—C10119.8 (3)
C22—P2—C3105.04 (15)C11—C10—P1118.3 (2)
C22—P2—C16105.67 (15)C11—C10—C15119.7 (3)
C16—P2—Pt1119.06 (10)C15—C10—P1121.5 (3)
C16—P2—C396.45 (15)C7—C6—C5119.9 (4)
C4—P1—Pt1110.94 (11)C13—C12—C11120.4 (4)
C4—P1—C1105.09 (15)C14—C15—C10119.5 (3)
C4—P1—C10105.47 (15)C22—C23—C24120.8 (3)
C1—P1—Pt1116.67 (11)C19—C20—C21120.8 (3)
C10—P1—Pt1120.83 (10)C6—C7—C8120.2 (4)
C10—P1—C195.82 (15)C12—C13—C14120.2 (3)
C9—C4—P1121.3 (3)C27—C26—C25120.2 (4)
C5—C4—P1119.5 (2)C25—C24—C23119.3 (4)
C5—C4—C9119.1 (3)C26—C27—C22120.0 (4)
C2—C3—P2115.8 (2)C26—C25—C24120.5 (4)
C17—C18—C19120.4 (3)Cl3B—C1B—Cl1B110.0 (2)
C2—C1—P1116.5 (2)Cl2B—C1B—Cl3B110.8 (2)
C20—C21—C16119.4 (3)Cl2B—C1B—Cl1B109.4 (2)
C1—C2—C3112.1 (3)Cl2A—C1A—Cl3A110.8 (2)
C8—C9—C4119.8 (3)Cl2A—C1A—Cl1A110.3 (2)
C23—C22—P2119.7 (2)Cl3A—C1A—Cl1A110.1 (2)
C23—C22—C27119.2 (3)Cl3C—C1C—Cl1C105.6 (5)
C27—C22—P2121.1 (3)Cl3C—C1C—Cl2C103.3 (5)
C13—C14—C15120.3 (3)Cl1C—C1C—Cl2C102.5 (6)
Pt1—P2—C3—C2−61.9 (3)C21—C16—C17—C181.2 (5)
Pt1—P2—C22—C23−19.8 (3)C9—C4—C5—C6−0.7 (5)
Pt1—P2—C22—C27162.4 (3)C9—C8—C7—C60.2 (6)
Pt1—P2—C16—C21−64.6 (3)C22—P2—C3—C263.2 (3)
Pt1—P2—C16—C17121.4 (2)C22—P2—C16—C21167.4 (3)
Pt1—P1—C4—C9−163.8 (2)C22—P2—C16—C17−6.6 (3)
Pt1—P1—C4—C519.2 (3)C22—C23—C24—C250.2 (6)
Pt1—P1—C1—C257.5 (3)C5—C4—C9—C80.8 (5)
Pt1—P1—C10—C1162.2 (3)C5—C6—C7—C8−0.1 (6)
Pt1—P1—C10—C15−125.6 (2)C16—P2—C3—C2171.3 (3)
P2—C3—C2—C172.9 (3)C16—P2—C22—C23111.8 (3)
P2—C22—C23—C24−177.6 (3)C16—P2—C22—C27−65.9 (3)
P2—C22—C27—C26177.6 (3)C16—C21—C20—C191.8 (5)
P2—C16—C17—C18175.1 (2)C19—C18—C17—C160.0 (5)
P1—C4—C9—C8−176.2 (3)C17—C18—C19—C20−0.3 (5)
P1—C4—C5—C6176.4 (3)C11—C10—C15—C140.2 (5)
P1—C1—C2—C3−70.5 (3)C11—C12—C13—C140.1 (6)
P1—C10—C15—C14−172.0 (2)C10—P1—C4—C963.7 (3)
C4—P1—C1—C2−65.8 (3)C10—P1—C4—C5−113.3 (3)
C4—P1—C10—C11−171.2 (2)C10—P1—C1—C2−173.6 (3)
C4—P1—C10—C151.1 (3)C10—C11—C12—C13−0.7 (6)
C4—C9—C8—C7−0.6 (6)C12—C11—C10—P1173.0 (3)
C4—C5—C6—C70.3 (6)C12—C11—C10—C150.6 (5)
C3—P2—C22—C23−146.9 (3)C15—C14—C13—C120.7 (6)
C3—P2—C22—C2735.4 (3)C23—C22—C27—C26−0.2 (5)
C3—P2—C16—C2159.8 (3)C23—C24—C25—C26−0.5 (6)
C3—P2—C16—C17−114.2 (3)C20—C21—C16—P2−176.1 (3)
C18—C19—C20—C21−0.6 (6)C20—C21—C16—C17−2.1 (5)
C1—P1—C4—C9−36.9 (3)C13—C14—C15—C10−0.8 (5)
C1—P1—C4—C5146.2 (3)C27—C22—C23—C240.2 (5)
C1—P1—C10—C11−63.7 (3)C27—C26—C25—C240.4 (7)
C1—P1—C10—C15108.5 (3)C25—C26—C27—C22−0.1 (6)
  4 in total

1.  A key step in the formation of acrylic acid from CO2 and ethylene: the transformation of a nickelalactone into a nickel-acrylate complex.

Authors:  Reinald Fischer; Jens Langer; Astrid Malassa; Dirk Walther; Helmar Görls; Gavin Vaughan
Journal:  Chem Commun (Camb)       Date:  2006-05-09       Impact factor: 6.222

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

3.  Using ligand bite angles to control the hydricity of palladium diphosphine complexes.

Authors:  James W Raebiger; Alex Miedaner; Calvin J Curtis; Susie M Miller; Oren P Anderson; Daniel L DuBois
Journal:  J Am Chem Soc       Date:  2004-05-05       Impact factor: 15.419

4.  Crystal structure refinement with SHELXL.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr C Struct Chem       Date:  2015-01-01       Impact factor: 1.172

  4 in total

北京卡尤迪生物科技股份有限公司 © 2022-2023.