Literature DB >> 21200586

Bis[1,2-bis-(dimethyl-phosphino)-ethane]-dichloridonitro-syltungsten(0) chloride.

Nataša Avramović1, Olivier Blacque, Helmut W Schmalle, Heinz Berke.   

Abstract

In the crystal structure of the title compound, [WCl(2)(NO)(C(6)H(16)P(2))(2)]Cl, the seven-coordinated tungsten(II) center displays a distorted penta-gonal-bipyramidal geometry with trans nitrosyl and chloride ligands. The NO and Cl ligands are disordered over two positions; the site occupancy factors are 0.6 and 0.4.

Entities:  

Year:  2007        PMID: 21200586      PMCID: PMC2915163          DOI: 10.1107/S1600536807067128

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


Related literature

For related trans-chloridonitrosyl-tungsten complexes, see: Chen et al. (2007 ▶). For related trans-chloridonitrosyl-bis­(1,2-bis­(dimethyl­phosphino)ethane)molybdenum complexes, see: Liang et al. (2003 ▶, 2006 ▶). For related literature, see: Bencze & Kohàn (1982 ▶); Carmona et al. (1989 ▶); Hunter & Legzdins (1984 ▶).

Experimental

Crystal data

[WCl2(NO)(C6H16P2)2]Cl M = 620.46 Monoclinic, a = 8.0929 (7) Å b = 26.118 (2) Å c = 10.5703 (10) Å β = 94.190 (10)° V = 2228.3 (3) Å3 Z = 4 Mo Kα radiation μ = 5.83 mm−1 T = 183 (2) K 0.20 × 0.15 × 0.07 mm

Data collection

Stoe IPDS diffractometer Absorption correction: numerical (Coppens et al., 1965 ▶) T min = 0.409, T max = 0.723 7761 measured reflections 3937 independent reflections 3353 reflections with I > 2σ(I) R int = 0.035

Refinement

R[F 2 > 2σ(F 2)] = 0.025 wR(F 2) = 0.060 S = 0.97 3937 reflections 217 parameters H-atom parameters constrained Δρmax = 0.83 e Å−3 Δρmin = −1.28 e Å−3 Data collection: IPDS Software (Stoe & Cie, 1999 ▶); cell refinement: IPDS Software; data reduction: X-RED in IPDS Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: PLATON (Spek, 2003 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536807067128/su2037sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536807067128/su2037Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[WCl2(NO)(C6H16P2)2]ClF000 = 1216
Mr = 620.46Dx = 1.850 Mg m3
Monoclinic, P21/nMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 8000 reflections
a = 8.0929 (7) Åθ = 2.4–28.0º
b = 26.118 (2) ŵ = 5.83 mm1
c = 10.5703 (10) ÅT = 183 (2) K
β = 94.190 (10)ºPlate, yellow
V = 2228.3 (3) Å30.20 × 0.15 × 0.07 mm
Z = 4
Stoe IPDS diffractometer3937 independent reflections
Radiation source: fine-focus sealed tube3353 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.035
T = 183(2) Kθmax = 25.0º
φ oscillation scanθmin = 2.5º
Absorption correction: numerical(Coppens et al., 1965)h = −9→9
Tmin = 0.410, Tmax = 0.723k = −30→30
7761 measured reflectionsl = 0→12
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.025H-atom parameters constrained
wR(F2) = 0.060  w = 1/[σ2(Fo2) + (0.0359P)2] where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max = 0.001
3937 reflectionsΔρmax = 0.83 e Å3
217 parametersΔρmin = −1.28 e Å3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
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)
W10.14034 (2)0.138353 (6)0.190758 (14)0.01228 (7)
P10.28028 (14)0.05181 (4)0.24110 (10)0.0148 (2)
P20.08089 (15)0.11528 (4)0.41984 (10)0.0187 (2)
P30.28985 (14)0.11874 (4)−0.00872 (10)0.0153 (2)
P40.05122 (15)0.20805 (4)0.02694 (10)0.0201 (2)
Cl1−0.03756 (17)0.20441 (5)0.28354 (11)0.0320 (3)
C10.1747 (6)0.01929 (18)0.3647 (4)0.0263 (11)
H1A0.06010.01040.33310.032*
H1B0.2337−0.01270.38980.032*
C20.1720 (6)0.05517 (19)0.4784 (4)0.0258 (11)
H2A0.28590.06100.51640.031*
H2B0.10500.04020.54380.031*
C30.4913 (6)0.0544 (2)0.3091 (4)0.0266 (11)
H3A0.53570.01960.31820.040*
H3B0.49410.07080.39260.040*
H3C0.55880.07420.25340.040*
C40.2717 (7)0.00030 (18)0.1264 (5)0.0311 (12)
H4A0.34300.00860.05810.047*
H4B0.1574−0.00410.09080.047*
H4C0.3102−0.03150.16810.047*
C50.1471 (7)0.1608 (2)0.5415 (5)0.0357 (13)
H5A0.09500.19400.52210.054*
H5B0.26790.16440.54470.054*
H5C0.11440.14860.62370.054*
C6−0.1376 (6)0.1041 (2)0.4354 (5)0.0323 (12)
H6A−0.15800.10160.52540.048*
H6B−0.17090.07200.39240.048*
H6C−0.20210.13250.39670.048*
C70.3072 (6)0.17713 (19)−0.1023 (4)0.0273 (11)
H7A0.38150.2019−0.05540.033*
H7B0.35460.1690−0.18370.033*
C80.1377 (6)0.19998 (19)−0.1269 (4)0.0273 (11)
H8A0.06640.1770−0.18180.033*
H8B0.14500.2335−0.17000.033*
C90.1887 (6)0.07605 (19)−0.1249 (4)0.0286 (11)
H9A0.25090.0755−0.20110.043*
H9B0.07570.0881−0.14730.043*
H9C0.18480.0415−0.08940.043*
C100.5051 (6)0.1013 (2)0.0067 (5)0.0287 (11)
H10A0.51690.06700.04350.043*
H10B0.56640.12590.06210.043*
H10C0.54950.1016−0.07710.043*
C110.1231 (7)0.27186 (18)0.0718 (5)0.0337 (12)
H11A0.09170.29590.00300.051*
H11B0.24400.27150.08760.051*
H11C0.07250.28260.14900.051*
C12−0.1699 (6)0.2108 (2)−0.0142 (5)0.0316 (12)
H12A−0.22820.21610.06270.047*
H12B−0.20660.1785−0.05450.047*
H12C−0.19440.2392−0.07320.047*
Cl30.54253 (16)0.09564 (5)0.66427 (11)0.0299 (3)
Cl21−0.0944 (3)0.08497 (11)0.1146 (2)0.0243 (8)0.597 (5)
N110.3280 (12)0.1748 (4)0.2417 (8)0.020 (2)0.597 (5)
O110.4639 (12)0.1916 (4)0.2679 (8)0.051 (3)0.597 (5)
Cl220.3926 (7)0.18470 (18)0.2565 (4)0.0243 (8)0.403 (5)
N12−0.0356 (16)0.0967 (5)0.1383 (12)0.020 (2)0.403 (5)
O12−0.1463 (16)0.0674 (6)0.1024 (13)0.051 (3)0.403 (5)
U11U22U33U12U13U23
W10.01609 (10)0.01170 (10)0.00949 (9)0.00126 (7)0.00396 (6)−0.00089 (6)
P10.0185 (6)0.0143 (5)0.0119 (5)0.0007 (4)0.0024 (4)0.0001 (4)
P20.0244 (6)0.0205 (6)0.0122 (5)−0.0016 (5)0.0078 (4)−0.0001 (4)
P30.0178 (6)0.0186 (6)0.0099 (5)0.0015 (4)0.0046 (4)0.0001 (4)
P40.0278 (7)0.0147 (6)0.0184 (6)0.0052 (5)0.0066 (5)0.0039 (4)
Cl10.0477 (8)0.0254 (6)0.0252 (6)0.0177 (6)0.0176 (5)0.0007 (5)
C10.033 (3)0.019 (2)0.027 (3)−0.002 (2)0.008 (2)0.005 (2)
C20.029 (3)0.032 (3)0.017 (2)−0.003 (2)0.0082 (19)0.0006 (19)
C30.021 (2)0.037 (3)0.022 (2)0.007 (2)−0.0004 (19)0.004 (2)
C40.051 (3)0.017 (2)0.025 (3)0.006 (2)−0.001 (2)−0.0013 (19)
C50.054 (4)0.032 (3)0.021 (2)−0.004 (3)0.003 (2)−0.006 (2)
C60.027 (3)0.037 (3)0.035 (3)0.001 (2)0.016 (2)0.006 (2)
C70.035 (3)0.027 (3)0.022 (2)−0.002 (2)0.011 (2)0.000 (2)
C80.041 (3)0.024 (3)0.017 (2)0.006 (2)0.004 (2)0.0076 (19)
C90.038 (3)0.030 (3)0.017 (2)0.001 (2)0.001 (2)−0.001 (2)
C100.023 (2)0.040 (3)0.025 (2)0.005 (2)0.0107 (19)0.002 (2)
C110.053 (3)0.014 (2)0.035 (3)−0.001 (2)0.009 (2)0.003 (2)
C120.031 (3)0.031 (3)0.033 (3)0.011 (2)0.004 (2)0.012 (2)
Cl30.0378 (7)0.0303 (7)0.0229 (6)0.0086 (5)0.0107 (5)0.0059 (5)
Cl210.016 (2)0.0332 (14)0.0231 (12)0.0016 (14)−0.0007 (12)−0.0017 (10)
N110.010 (5)0.034 (4)0.017 (4)−0.002 (4)0.004 (3)−0.002 (3)
O110.027 (5)0.073 (5)0.052 (4)−0.004 (4)−0.006 (4)−0.018 (4)
Cl220.016 (2)0.0332 (14)0.0231 (12)0.0016 (14)−0.0007 (12)−0.0017 (10)
N120.010 (5)0.034 (4)0.017 (4)−0.002 (4)0.004 (3)−0.002 (3)
O120.027 (5)0.073 (5)0.052 (4)−0.004 (4)−0.006 (4)−0.018 (4)
W1—P12.5665 (11)C3—H3B0.9800
W1—P22.5745 (11)C3—H3C0.9800
W1—P32.5583 (11)C4—H4A0.9800
W1—P42.5788 (11)C4—H4B0.9800
W1—Cl12.4935 (11)C4—H4C0.9800
W1—Cl212.445 (3)C5—H5A0.9800
W1—Cl222.431 (5)C5—H5B0.9800
W1—N111.840 (11)C5—H5C0.9800
W1—N121.845 (13)C6—H6A0.9800
N11—O111.198 (15)C6—H6B0.9800
N12—O121.218 (17)C6—H6C0.9800
P1—C31.805 (5)C7—C81.502 (7)
P1—C41.809 (5)C7—H7A0.9900
P1—C11.823 (5)C7—H7B0.9900
P2—C51.803 (5)C8—H8A0.9900
P2—C61.812 (5)C8—H8B0.9900
P2—C21.823 (5)C9—H9A0.9800
P3—C101.796 (5)C9—H9B0.9800
P3—C91.810 (5)C9—H9C0.9800
P3—C71.829 (5)C10—H10A0.9800
P4—C121.812 (5)C10—H10B0.9800
P4—C111.817 (5)C10—H10C0.9800
P4—C81.829 (5)C11—H11A0.9800
C1—C21.525 (7)C11—H11B0.9800
C1—H1A0.9900C11—H11C0.9800
C1—H1B0.9900C12—H12A0.9800
C2—H2A0.9900C12—H12B0.9800
C2—H2B0.9900C12—H12C0.9800
C3—H3A0.9800
N11—W1—N12174.8 (4)P2—C2—H2A110.3
N11—W1—Cl21175.3 (3)C1—C2—H2B110.3
N12—W1—Cl22173.3 (5)P2—C2—H2B110.3
Cl22—W1—Cl21173.87 (10)H2A—C2—H2B108.6
N11—W1—Cl190.8 (3)P1—C3—H3A109.5
N12—W1—Cl194.1 (4)P1—C3—H3B109.5
Cl21—W1—Cl193.84 (7)H3A—C3—H3B109.5
Cl22—W1—Cl192.29 (11)P1—C3—H3C109.5
N11—W1—P385.1 (2)H3A—C3—H3C109.5
N12—W1—P392.0 (4)H3B—C3—H3C109.5
Cl22—W1—P384.12 (11)P1—C4—H4A109.5
Cl21—W1—P391.00 (6)P1—C4—H4B109.5
Cl1—W1—P3141.64 (4)H4A—C4—H4B109.5
N11—W1—P193.0 (3)P1—C4—H4C109.5
N12—W1—P182.1 (4)H4A—C4—H4C109.5
Cl22—W1—P191.76 (11)H4B—C4—H4C109.5
Cl21—W1—P183.48 (6)P2—C5—H5A109.5
Cl1—W1—P1141.86 (4)P2—C5—H5B109.5
P1—W1—P273.07 (4)H5A—C5—H5B109.5
P1—W1—P376.49 (3)P2—C5—H5C109.5
N11—W1—P293.0 (3)H5A—C5—H5C109.5
N12—W1—P287.2 (4)H5B—C5—H5C109.5
Cl22—W1—P293.34 (11)P2—C6—H6A109.5
Cl21—W1—P288.97 (6)P2—C6—H6B109.5
Cl1—W1—P268.84 (4)H6A—C6—H6B109.5
P3—W1—P2149.37 (4)P2—C6—H6C109.5
N11—W1—P490.9 (3)H6A—C6—H6C109.5
N12—W1—P492.5 (4)H6B—C6—H6C109.5
Cl22—W1—P491.62 (11)C8—C7—P3108.6 (3)
Cl21—W1—P490.52 (7)C8—C7—H7A110.0
Cl1—W1—P468.56 (4)P3—C7—H7A110.0
P3—W1—P473.37 (4)C8—C7—H7B110.0
P1—W1—P4149.15 (3)P3—C7—H7B110.0
P2—W1—P4137.26 (4)H7A—C7—H7B108.3
C3—P1—C4106.5 (2)C7—C8—P4107.2 (3)
C3—P1—C1102.2 (2)C7—C8—H8A110.3
C4—P1—C197.9 (2)P4—C8—H8A110.3
C3—P1—W1116.09 (17)C7—C8—H8B110.3
C4—P1—W1121.42 (16)P4—C8—H8B110.3
C1—P1—W1109.64 (16)H8A—C8—H8B108.5
C5—P2—C6106.4 (3)P3—C9—H9A109.5
C5—P2—C2103.5 (2)P3—C9—H9B109.5
C6—P2—C2101.7 (2)H9A—C9—H9B109.5
C5—P2—W1116.77 (18)P3—C9—H9C109.5
C6—P2—W1111.95 (17)H9A—C9—H9C109.5
C2—P2—W1114.95 (15)H9B—C9—H9C109.5
C10—P3—C9107.0 (2)P3—C10—H10A109.5
C10—P3—C798.5 (2)P3—C10—H10B109.5
C9—P3—C7101.3 (2)H10A—C10—H10B109.5
C10—P3—W1119.33 (16)P3—C10—H10C109.5
C9—P3—W1117.72 (17)H10A—C10—H10C109.5
C7—P3—W1109.79 (16)H10B—C10—H10C109.5
C12—P4—C11108.6 (3)P4—C11—H11A109.5
C12—P4—C8103.1 (2)P4—C11—H11B109.5
C11—P4—C8101.6 (2)H11A—C11—H11B109.5
C12—P4—W1114.33 (17)P4—C11—H11C109.5
C11—P4—W1113.81 (17)H11A—C11—H11C109.5
C8—P4—W1114.16 (15)H11B—C11—H11C109.5
C2—C1—P1108.2 (3)P4—C12—H12A109.5
C2—C1—H1A110.1P4—C12—H12B109.5
P1—C1—H1A110.1H12A—C12—H12B109.5
C2—C1—H1B110.1P4—C12—H12C109.5
P1—C1—H1B110.1H12A—C12—H12C109.5
H1A—C1—H1B108.4H12B—C12—H12C109.5
C1—C2—P2106.9 (3)O11—N11—W1169.1 (8)
C1—C2—H2A110.3O12—N12—W1176.9 (15)
N11—W1—P1—C32.3 (3)Cl22—W1—P3—C9175.1 (2)
N12—W1—P1—C3−179.4 (4)Cl21—W1—P3—C9−1.2 (2)
Cl22—W1—P1—C33.0 (2)Cl1—W1—P3—C9−98.7 (2)
Cl21—W1—P1—C3179.16 (18)P1—W1—P3—C981.82 (19)
Cl1—W1—P1—C3−92.92 (18)P2—W1—P3—C988.4 (2)
P3—W1—P1—C386.56 (18)P4—W1—P3—C9−91.47 (19)
P2—W1—P1—C3−89.93 (18)N11—W1—P3—C7−68.8 (3)
P4—W1—P1—C399.15 (18)N12—W1—P3—C7115.6 (5)
N11—W1—P1—C4−129.7 (3)Cl22—W1—P3—C7−69.9 (2)
N12—W1—P1—C448.6 (5)Cl21—W1—P3—C7113.84 (19)
Cl22—W1—P1—C4−128.9 (3)Cl1—W1—P3—C716.37 (19)
Cl21—W1—P1—C447.2 (2)P1—W1—P3—C7−163.11 (18)
Cl1—W1—P1—C4135.1 (2)P2—W1—P3—C7−156.49 (18)
P3—W1—P1—C4−45.4 (2)P4—W1—P3—C723.60 (18)
P2—W1—P1—C4138.1 (2)N11—W1—P4—C12−154.6 (3)
P4—W1—P1—C4−32.8 (2)N12—W1—P4—C1229.4 (5)
N11—W1—P1—C1117.5 (3)Cl22—W1—P4—C12−155.9 (2)
N12—W1—P1—C1−64.3 (4)Cl21—W1—P4—C1229.8 (2)
Cl22—W1—P1—C1118.2 (2)Cl1—W1—P4—C12−64.1 (2)
Cl21—W1—P1—C1−65.69 (18)P3—W1—P4—C12120.7 (2)
Cl1—W1—P1—C122.23 (19)P1—W1—P4—C12107.9 (2)
P3—W1—P1—C1−158.29 (17)P2—W1—P4—C12−59.2 (2)
P2—W1—P1—C125.23 (17)N11—W1—P4—C11−29.1 (3)
P4—W1—P1—C1−145.69 (18)N12—W1—P4—C11154.9 (5)
N11—W1—P2—C530.3 (3)Cl22—W1—P4—C11−30.3 (2)
N12—W1—P2—C5−154.9 (5)Cl21—W1—P4—C11155.4 (2)
Cl22—W1—P2—C531.7 (2)Cl1—W1—P4—C1161.5 (2)
Cl21—W1—P2—C5−153.9 (2)P3—W1—P4—C11−113.7 (2)
Cl1—W1—P2—C5−59.4 (2)P1—W1—P4—C11−126.5 (2)
P3—W1—P2—C5115.8 (2)P2—W1—P4—C1166.4 (2)
P1—W1—P2—C5122.6 (2)N11—W1—P4—C887.0 (3)
P4—W1—P2—C5−64.3 (2)N12—W1—P4—C8−89.0 (4)
N11—W1—P2—C6153.4 (3)Cl22—W1—P4—C885.7 (2)
N12—W1—P2—C6−31.9 (5)Cl21—W1—P4—C8−88.5 (2)
Cl22—W1—P2—C6154.8 (2)Cl1—W1—P4—C8177.56 (19)
Cl21—W1—P2—C6−30.9 (2)P3—W1—P4—C82.37 (19)
Cl1—W1—P2—C663.6 (2)P1—W1—P4—C8−10.4 (2)
P3—W1—P2—C6−121.1 (2)P2—W1—P4—C8−177.56 (19)
P1—W1—P2—C6−114.4 (2)C3—P1—C1—C268.8 (4)
P4—W1—P2—C658.8 (2)C4—P1—C1—C2177.6 (4)
N11—W1—P2—C2−91.2 (3)W1—P1—C1—C2−54.9 (4)
N12—W1—P2—C283.6 (5)P1—C1—C2—P253.9 (4)
Cl22—W1—P2—C2−89.8 (2)C5—P2—C2—C1−160.7 (3)
Cl21—W1—P2—C284.53 (19)C6—P2—C2—C189.0 (4)
Cl1—W1—P2—C2179.05 (18)W1—P2—C2—C1−32.2 (4)
P3—W1—P2—C2−5.7 (2)C10—P3—C7—C8−179.3 (3)
P1—W1—P2—C21.03 (18)C9—P3—C7—C871.3 (4)
P4—W1—P2—C2174.18 (18)W1—P3—C7—C8−53.8 (3)
N11—W1—P3—C1043.7 (3)P3—C7—C8—P454.2 (4)
N12—W1—P3—C10−132.0 (5)C12—P4—C8—C7−158.3 (3)
Cl22—W1—P3—C1042.6 (2)C11—P4—C8—C789.3 (4)
Cl21—W1—P3—C10−133.7 (2)W1—P4—C8—C7−33.7 (4)
Cl1—W1—P3—C10128.8 (2)Cl22—W1—N11—O112(10)
P1—W1—P3—C10−50.6 (2)Cl1—W1—N11—O11174 (4)
P2—W1—P3—C10−44.0 (2)P3—W1—N11—O11−44 (4)
P4—W1—P3—C10136.1 (2)P1—W1—N11—O1132 (4)
N11—W1—P3—C9176.1 (3)P2—W1—N11—O11105 (4)
N12—W1—P3—C90.5 (5)P4—W1—N11—O11−118 (4)
W1—P12.5665 (11)
W1—P22.5745 (11)
W1—P32.5583 (11)
W1—P42.5788 (11)
W1—Cl12.4935 (11)
W1—Cl212.445 (3)
W1—Cl222.431 (5)
W1—N111.840 (11)
W1—N121.845 (13)
P1—W1—P273.07 (4)
P1—W1—P376.49 (3)
Cl1—W1—P268.84 (4)
Cl1—W1—P468.56 (4)
P3—W1—P473.37 (4)
  1 in total

1.  μ-1,2-Bis(diethyl-phosphino)ethane-κP:P'-bis-{[1,2-bis-(diethyl-phosphino)ethane-κP,P']trichloridonitrosyl-tungsten(II)}.

Authors:  Nataša Avramović; Olivier Blacque; Helmut W Schmalle; Heinz Berke
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2008-01-16
  1 in total

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