Literature DB >> 22199590

Bis{1,2-bis-[bis-(3-meth-oxy-prop-yl)phosphan-yl]ethane-κP,P'}dichlorido-osmium(II).

Nathaniel K Szymczak1, Lev N Zakharov, David R Tyler.   

Abstract

In the centrosymmetric title compound, [OsCl(2)(C(18)H(40)O(4)P(2))(2)], the Os(II) atom adopts a trans-OsCl(2)P(4) geometry, arising from its coordination by two chelating diphosphane ligands and two chloride ions. One of the meth-oxy side chains of the ligand is disordered over two orientations in a 0.700 (6):0.300 (6) ratio.

Entities:  

Year:  2011        PMID: 22199590      PMCID: PMC3238713          DOI: 10.1107/S1600536811048926

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For background to transition-metal dihydride complexes, see: Egbert et al. (2007 ▶); Heinekey et al. (2004 ▶); Miller et al. (2002 ▶); Szymczak & Tyler (2007 ▶); Szymczak et al. (2006 ▶).

Experimental

Crystal data

[OsCl2(C18H40O4P2)2] M = 1025.98 Monoclinic, a = 12.667 (3) Å b = 10.321 (2) Å c = 18.754 (4) Å β = 107.779 (3)° V = 2335.0 (9) Å3 Z = 2 Mo Kα radiation μ = 3.03 mm−1 T = 173 K 0.14 × 0.10 × 0.04 mm

Data collection

Bruker APEX CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1995 ▶) T min = 0.677, T max = 0.889 25950 measured reflections 5333 independent reflections 4423 reflections with I > 2σ(I) R int = 0.032

Refinement

R[F 2 > 2σ(F 2)] = 0.024 wR(F 2) = 0.058 S = 1.04 5333 reflections 251 parameters 5 restraints H-atom parameters constrained Δρmax = 0.87 e Å−3 Δρmin = −0.51 e Å−3 Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT (Bruker, 2000 ▶); program(s) used to solve structure: SHELXTL (Sheldrick, 2008) ▶; program(s) used to refine structure: SHELXTL (Sheldrick, 2008) ▶; molecular graphics: SHELXTL (Sheldrick, 2008) ▶; software used to prepare material for publication: SHELXTL (Sheldrick, 2008) ▶. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811048926/hb6479sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811048926/hb6479Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[OsCl2(C18H40O4P2)2]F(000) = 1060
Mr = 1025.98Dx = 1.459 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 8415 reflections
a = 12.667 (3) Åθ = 2.3–26.7°
b = 10.321 (2) ŵ = 3.03 mm1
c = 18.754 (4) ÅT = 173 K
β = 107.779 (3)°Plate, yellow
V = 2335.0 (9) Å30.14 × 0.10 × 0.04 mm
Z = 2
Bruker APEX CCD diffractometer5333 independent reflections
Radiation source: fine-focus sealed tube4423 reflections with I > 2σ(I)
graphiteRint = 0.032
phi and ω scansθmax = 27.5°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1995)h = −16→16
Tmin = 0.677, Tmax = 0.889k = −13→13
25950 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)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.058H-atom parameters constrained
S = 1.04w = 1/[σ2(Fo2) + (0.028P)2 + 0.9782P] where P = (Fo2 + 2Fc2)/3
5333 reflections(Δ/σ)max < 0.001
251 parametersΔρmax = 0.87 e Å3
5 restraintsΔρmin = −0.51 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 takeninto account individually in the estimation of e.s.d.'s in distances, anglesand torsion angles; correlations between e.s.d.'s in cell parameters are onlyused 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)
Os10.50000.50000.00000.02110 (5)
Cl10.31396 (6)0.41077 (7)−0.05728 (4)0.03191 (16)
P10.57375 (6)0.32518 (7)−0.04887 (4)0.02556 (15)
P20.53170 (6)0.36384 (7)0.10408 (4)0.02567 (15)
O10.9493 (2)0.2799 (3)−0.02252 (14)0.0575 (7)
O20.5043 (2)0.1314 (3)−0.27322 (14)0.0666 (8)
O30.5690 (2)0.4496 (3)0.35068 (13)0.0512 (6)
C10.5965 (3)0.1882 (3)0.01729 (16)0.0354 (7)
H1A0.52700.13840.00890.043*
H1B0.65390.12950.00960.043*
C20.6341 (3)0.2421 (3)0.09683 (16)0.0352 (7)
H2A0.70820.28230.10760.042*
H2B0.63860.17150.13340.042*
C30.7111 (2)0.3487 (3)−0.05918 (18)0.0355 (7)
H3A0.70850.4293−0.08830.043*
H3B0.76320.3645−0.00860.043*
C40.7620 (3)0.2440 (3)−0.09552 (18)0.0397 (7)
H4A0.76570.1617−0.06770.048*
H4B0.71410.2298−0.14750.048*
C50.8773 (3)0.2810 (4)−0.09625 (19)0.0457 (8)
H5A0.90350.2188−0.12730.055*
H5B0.87590.3685−0.11820.055*
C61.0568 (3)0.3250 (5)−0.0175 (2)0.0691 (12)
H6A1.10370.32190.03480.104*
H6B1.05210.4144−0.03580.104*
H6C1.08890.2699−0.04810.104*
C70.4913 (3)0.2555 (3)−0.13885 (17)0.0336 (7)
H7A0.41270.2782−0.14650.040*
H7B0.51400.2990−0.17890.040*
C80.4975 (3)0.1093 (3)−0.15003 (18)0.0410 (8)
H8A0.57610.0816−0.13390.049*
H8B0.45930.0638−0.11850.049*
C90.4444 (3)0.0725 (3)−0.23097 (19)0.0455 (8)
H9A0.4455−0.0228−0.23670.055*
H9B0.36640.1021−0.24810.055*
C100.4635 (4)0.1030 (6)−0.3488 (2)0.0944 (18)
H10A0.50890.1464−0.37550.142*
H10B0.38670.1333−0.36830.142*
H10C0.46590.0091−0.35600.142*
C110.5917 (2)0.4287 (3)0.19857 (16)0.0303 (6)
H11A0.65540.48420.19840.036*
H11B0.53560.48530.20970.036*
C120.6318 (3)0.3317 (3)0.26298 (17)0.0381 (7)
H12A0.57180.26900.26080.046*
H12B0.69590.28290.25710.046*
C130.6655 (3)0.3987 (3)0.33861 (18)0.0437 (8)
H13A0.70160.33610.37860.052*
H13B0.71870.46930.33930.052*
C140.5931 (5)0.5225 (4)0.4180 (3)0.0833 (16)
H14A0.52400.55590.42410.125*
H14B0.64190.59500.41570.125*
H14C0.63010.46670.46060.125*
C150.4218 (3)0.2540 (3)0.11326 (17)0.0374 (7)
H15A0.38100.22110.06280.045*
H15B0.45770.17870.14380.045*
C160.3385 (3)0.3093 (3)0.1475 (2)0.0509 (9)
H16A0.29350.37630.11400.061*
H16B0.37770.35080.19600.061*
C170.2609 (4)0.2002 (6)0.1602 (3)0.0890 (18)0.700 (6)
H17A0.19750.23960.17270.107*0.700 (6)
H17B0.23130.14950.11360.107*0.700 (6)
O40.3138 (3)0.1245 (3)0.2135 (2)0.0515 (12)0.700 (6)
C180.2400 (6)0.0305 (5)0.2282 (4)0.0579 (17)0.700 (6)
H18A0.2813−0.02640.26900.087*0.700 (6)
H18B0.2072−0.02130.18300.087*0.700 (6)
H18C0.18120.07470.24260.087*0.700 (6)
C17A0.2609 (4)0.2002 (6)0.1602 (3)0.0890 (18)0.300 (6)
H17C0.21400.17210.11010.107*0.300 (6)
H17D0.30900.12570.18250.107*0.300 (6)
O4A0.2061 (9)0.2156 (9)0.1940 (6)0.072 (4)0.300 (6)
C18A0.1540 (15)0.0978 (17)0.2088 (10)0.098 (7)0.300 (6)
H18D0.10480.11840.23870.146*0.300 (6)
H18E0.21120.03680.23640.146*0.300 (6)
H18F0.11060.05860.16120.146*0.300 (6)
U11U22U33U12U13U23
Os10.02079 (8)0.01550 (8)0.02816 (8)−0.00026 (6)0.00918 (6)0.00023 (6)
Cl10.0249 (3)0.0302 (4)0.0410 (4)−0.0056 (3)0.0105 (3)−0.0045 (3)
P10.0281 (4)0.0187 (3)0.0315 (4)0.0028 (3)0.0115 (3)0.0000 (3)
P20.0300 (4)0.0183 (3)0.0300 (4)0.0004 (3)0.0112 (3)0.0013 (3)
O10.0332 (13)0.091 (2)0.0499 (15)0.0038 (14)0.0149 (11)0.0043 (14)
O20.080 (2)0.078 (2)0.0400 (14)−0.0198 (16)0.0150 (14)−0.0137 (14)
O30.0617 (17)0.0534 (14)0.0407 (14)−0.0105 (13)0.0189 (12)−0.0129 (12)
C10.0489 (19)0.0217 (15)0.0398 (17)0.0087 (13)0.0196 (15)0.0028 (13)
C20.0464 (18)0.0263 (15)0.0345 (16)0.0116 (13)0.0146 (14)0.0071 (12)
C30.0338 (16)0.0309 (16)0.0464 (18)0.0029 (13)0.0188 (14)−0.0018 (14)
C40.0377 (18)0.0457 (19)0.0392 (18)0.0094 (15)0.0169 (15)−0.0033 (15)
C50.0375 (18)0.060 (2)0.047 (2)0.0101 (16)0.0230 (16)−0.0002 (17)
C60.036 (2)0.097 (4)0.074 (3)0.004 (2)0.016 (2)−0.002 (3)
C70.0354 (17)0.0254 (15)0.0382 (17)0.0027 (12)0.0088 (14)−0.0059 (13)
C80.057 (2)0.0219 (16)0.0427 (18)−0.0017 (14)0.0134 (16)−0.0029 (13)
C90.051 (2)0.0304 (18)0.050 (2)−0.0037 (15)0.0078 (17)−0.0116 (15)
C100.074 (3)0.160 (6)0.044 (3)0.007 (3)0.011 (2)−0.018 (3)
C110.0334 (16)0.0243 (16)0.0323 (15)0.0008 (12)0.0086 (13)0.0014 (12)
C120.0465 (19)0.0299 (17)0.0347 (16)0.0052 (14)0.0074 (14)0.0044 (13)
C130.051 (2)0.0391 (19)0.0338 (17)−0.0034 (16)0.0019 (15)0.0051 (14)
C140.115 (5)0.076 (3)0.061 (3)−0.019 (3)0.031 (3)−0.033 (2)
C150.0468 (19)0.0304 (17)0.0363 (17)−0.0084 (14)0.0148 (15)0.0023 (13)
C160.046 (2)0.048 (2)0.065 (2)−0.0052 (17)0.0256 (18)0.0135 (18)
C170.080 (3)0.128 (5)0.076 (3)0.005 (3)0.048 (3)0.044 (3)
O40.041 (2)0.058 (2)0.056 (2)−0.0074 (17)0.0166 (17)0.0144 (18)
C180.059 (4)0.047 (3)0.080 (4)−0.018 (3)0.042 (4)0.005 (3)
C17A0.080 (3)0.128 (5)0.076 (3)0.005 (3)0.048 (3)0.044 (3)
O4A0.077 (7)0.062 (6)0.077 (7)−0.007 (5)0.024 (6)0.012 (5)
C18A0.076 (12)0.099 (14)0.105 (13)−0.061 (11)0.009 (10)0.042 (11)
Os1—P22.3383 (8)C8—C91.509 (4)
Os1—P2i2.3383 (8)C8—H8A0.9900
Os1—P1i2.3434 (8)C8—H8B0.9900
Os1—P12.3434 (8)C9—H9A0.9900
Os1—Cl12.4515 (8)C9—H9B0.9900
Os1—Cl1i2.4515 (8)C10—H10A0.9800
P1—C31.825 (3)C10—H10B0.9800
P1—C71.838 (3)C10—H10C0.9800
P1—C11.845 (3)C11—C121.531 (4)
P2—C111.829 (3)C11—H11A0.9900
P2—C21.840 (3)C11—H11B0.9900
P2—C151.844 (3)C12—C131.517 (4)
O1—C51.405 (4)C12—H12A0.9900
O1—C61.414 (4)C12—H12B0.9900
O2—C101.384 (5)C13—H13A0.9900
O2—C91.392 (4)C13—H13B0.9900
O3—C131.412 (4)C14—H14A0.9800
O3—C141.420 (5)C14—H14B0.9800
C1—C21.525 (4)C14—H14C0.9800
C1—H1A0.9900C15—C161.506 (5)
C1—H1B0.9900C15—H15A0.9900
C2—H2A0.9900C15—H15B0.9900
C2—H2B0.9900C16—C171.560 (6)
C3—C41.521 (4)C16—H16A0.9900
C3—H3A0.9900C16—H16B0.9900
C3—H3B0.9900C17—O41.283 (5)
C4—C51.514 (4)C17—H17A0.9900
C4—H4A0.9900C17—H17B0.9900
C4—H4B0.9900O4—C181.431 (6)
C5—H5A0.9900C18—H18A0.9800
C5—H5B0.9900C18—H18B0.9800
C6—H6A0.9800C18—H18C0.9800
C6—H6B0.9800O4A—C18A1.451 (13)
C6—H6C0.9800C18A—H18D0.9800
C7—C81.528 (4)C18A—H18E0.9800
C7—H7A0.9900C18A—H18F0.9800
C7—H7B0.9900
P2—Os1—P2i180.00 (4)C9—C8—H8A109.4
P2—Os1—P1i97.10 (3)C7—C8—H8A109.4
P2i—Os1—P1i82.90 (3)C9—C8—H8B109.4
P2—Os1—P182.90 (3)C7—C8—H8B109.4
P2i—Os1—P197.10 (3)H8A—C8—H8B108.0
P1i—Os1—P1180.00 (3)O2—C9—C8108.1 (3)
P2—Os1—Cl192.13 (3)O2—C9—H9A110.1
P2i—Os1—Cl187.87 (3)C8—C9—H9A110.1
P1i—Os1—Cl190.91 (3)O2—C9—H9B110.1
P1—Os1—Cl189.09 (3)C8—C9—H9B110.1
P2—Os1—Cl1i87.87 (3)H9A—C9—H9B108.4
P2i—Os1—Cl1i92.13 (3)O2—C10—H10A109.5
P1i—Os1—Cl1i89.09 (3)O2—C10—H10B109.5
P1—Os1—Cl1i90.91 (3)H10A—C10—H10B109.5
Cl1—Os1—Cl1i180.0O2—C10—H10C109.5
C3—P1—C7104.32 (15)H10A—C10—H10C109.5
C3—P1—C1102.40 (15)H10B—C10—H10C109.5
C7—P1—C1104.24 (14)C12—C11—P2117.7 (2)
C3—P1—Os1116.50 (10)C12—C11—H11A107.9
C7—P1—Os1118.55 (10)P2—C11—H11A107.9
C1—P1—Os1109.03 (10)C12—C11—H11B107.9
C11—P2—C2103.16 (14)P2—C11—H11B107.9
C11—P2—C15103.69 (14)H11A—C11—H11B107.2
C2—P2—C1598.98 (15)C13—C12—C11111.8 (2)
C11—P2—Os1120.25 (10)C13—C12—H12A109.3
C2—P2—Os1107.11 (10)C11—C12—H12A109.3
C15—P2—Os1120.36 (11)C13—C12—H12B109.3
C5—O1—C6112.7 (3)C11—C12—H12B109.3
C10—O2—C9113.1 (3)H12A—C12—H12B107.9
C13—O3—C14112.2 (3)O3—C13—C12108.0 (3)
C2—C1—P1108.5 (2)O3—C13—H13A110.1
C2—C1—H1A110.0C12—C13—H13A110.1
P1—C1—H1A110.0O3—C13—H13B110.1
C2—C1—H1B110.0C12—C13—H13B110.1
P1—C1—H1B110.0H13A—C13—H13B108.4
H1A—C1—H1B108.4O3—C14—H14A109.5
C1—C2—P2107.7 (2)O3—C14—H14B109.5
C1—C2—H2A110.2H14A—C14—H14B109.5
P2—C2—H2A110.2O3—C14—H14C109.5
C1—C2—H2B110.2H14A—C14—H14C109.5
P2—C2—H2B110.2H14B—C14—H14C109.5
H2A—C2—H2B108.5C16—C15—P2117.0 (2)
C4—C3—P1120.1 (2)C16—C15—H15A108.0
C4—C3—H3A107.3P2—C15—H15A108.0
P1—C3—H3A107.3C16—C15—H15B108.0
C4—C3—H3B107.3P2—C15—H15B108.0
P1—C3—H3B107.3H15A—C15—H15B107.3
H3A—C3—H3B106.9C15—C16—C17110.3 (3)
C5—C4—C3111.5 (3)C15—C16—H16A109.6
C5—C4—H4A109.3C17—C16—H16A109.6
C3—C4—H4A109.3C15—C16—H16B109.6
C5—C4—H4B109.3C17—C16—H16B109.6
C3—C4—H4B109.3H16A—C16—H16B108.1
H4A—C4—H4B108.0O4—C17—C16110.8 (4)
O1—C5—C4109.1 (3)O4—C17—H17A109.5
O1—C5—H5A109.9C16—C17—H17A109.5
C4—C5—H5A109.9O4—C17—H17B109.5
O1—C5—H5B109.9C16—C17—H17B109.5
C4—C5—H5B109.9H17A—C17—H17B108.1
H5A—C5—H5B108.3C17—O4—C18110.3 (4)
O1—C6—H6A109.5O4—C18—H18A109.5
O1—C6—H6B109.5O4—C18—H18B109.5
H6A—C6—H6B109.5H18A—C18—H18B109.5
O1—C6—H6C109.5O4—C18—H18C109.5
H6A—C6—H6C109.5H18A—C18—H18C109.5
H6B—C6—H6C109.5H18B—C18—H18C109.5
C8—C7—P1118.3 (2)O4A—C18A—H18D109.5
C8—C7—H7A107.7O4A—C18A—H18E109.5
P1—C7—H7A107.7H18D—C18A—H18E109.5
C8—C7—H7B107.7O4A—C18A—H18F109.5
P1—C7—H7B107.7H18D—C18A—H18F109.5
H7A—C7—H7B107.1H18E—C18A—H18F109.5
C9—C8—C7111.2 (3)
P2—Os1—P1—C3−109.55 (12)C7—P1—C1—C2−163.7 (2)
P2i—Os1—P1—C370.45 (12)Os1—P1—C1—C2−36.2 (2)
P1i—Os1—P1—C35(47)P1—C1—C2—P253.3 (2)
Cl1—Os1—P1—C3158.19 (12)C11—P2—C2—C1−175.8 (2)
Cl1i—Os1—P1—C3−21.81 (12)C15—P2—C2—C177.8 (2)
P2—Os1—P1—C7124.59 (12)Os1—P2—C2—C1−47.9 (2)
P2i—Os1—P1—C7−55.41 (12)C7—P1—C3—C4−43.0 (3)
P1i—Os1—P1—C7−121 (47)C1—P1—C3—C465.5 (3)
Cl1—Os1—P1—C732.34 (12)Os1—P1—C3—C4−175.7 (2)
Cl1i—Os1—P1—C7−147.66 (12)P1—C3—C4—C5−178.2 (2)
P2—Os1—P1—C15.65 (11)C6—O1—C5—C4−174.6 (3)
P2i—Os1—P1—C1−174.35 (11)C3—C4—C5—O168.8 (4)
P1i—Os1—P1—C1120 (47)C3—P1—C7—C883.9 (3)
Cl1—Os1—P1—C1−86.61 (11)C1—P1—C7—C8−23.2 (3)
Cl1i—Os1—P1—C193.39 (11)Os1—P1—C7—C8−144.6 (2)
P2i—Os1—P2—C1188 (100)P1—C7—C8—C9−168.4 (2)
P1i—Os1—P2—C11−43.13 (12)C10—O2—C9—C8179.3 (4)
P1—Os1—P2—C11136.87 (12)C7—C8—C9—O262.8 (4)
Cl1—Os1—P2—C11−134.31 (12)C2—P2—C11—C12−49.0 (3)
Cl1i—Os1—P2—C1145.69 (12)C15—P2—C11—C1253.8 (3)
P2i—Os1—P2—C2−29 (100)Os1—P2—C11—C12−168.09 (19)
P1i—Os1—P2—C2−160.21 (11)P2—C11—C12—C13−172.6 (2)
P1—Os1—P2—C219.79 (11)C14—O3—C13—C12−175.8 (3)
Cl1—Os1—P2—C2108.61 (11)C11—C12—C13—O368.3 (3)
Cl1i—Os1—P2—C2−71.39 (11)C11—P2—C15—C1652.9 (3)
P2i—Os1—P2—C15−141 (100)C2—P2—C15—C16158.9 (3)
P1i—Os1—P2—C1588.10 (12)Os1—P2—C15—C16−85.1 (3)
P1—Os1—P2—C15−91.90 (12)P2—C15—C16—C17−173.0 (3)
Cl1—Os1—P2—C15−3.08 (12)C15—C16—C17—O470.8 (5)
Cl1i—Os1—P2—C15176.92 (12)C16—C17—O4—C18175.9 (4)
C3—P1—C1—C287.8 (2)
Table 1

Selected bond lengths (Å)

Os1—P22.3383 (8)
Os1—P12.3434 (8)
Os1—Cl12.4515 (8)
  4 in total

1.  Elongated dihydrogen complexes: what remains of the H-H bond?

Authors:  D Michael Heinekey; Agustí Lledŏs; José M Lluch
Journal:  Chem Soc Rev       Date:  2004-02-27       Impact factor: 54.564

2.  A short history of SHELX.

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

3.  Solution chemistry of a water-soluble eta2-H2 ruthenium complex: evidence for coordinated H2 acting as a hydrogen bond donor.

Authors:  Nathaniel K Szymczak; Lev N Zakharov; David R Tyler
Journal:  J Am Chem Soc       Date:  2006-12-13       Impact factor: 15.419

4.  Precursors to water-soluble dinitrogen carriers. Synthesis of water-soluble complexes of iron(II) containing water-soluble chelating phosphine ligands of the type 1,2-bis(bis(hydroxyalkyl)phosphino)ethane.

Authors:  Warren K Miller; John D Gilbertson; Carmen Leiva-Paredes; Paul R Bernatis; Timothy J R Weakley; David K Lyon; David R Tyler
Journal:  Inorg Chem       Date:  2002-10-21       Impact factor: 5.165

  4 in total

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