Literature DB >> 21201325

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

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

Abstract

The title binuclear compound, [W(2)Cl(6)(NO)(2)(C(10)H(22)P(2))(3)], contains two W atoms which are bridged by a bis-(diethyl-phosphino)-ethane (depe) ligand. The seven-coord-inated tungsten(II) centres display distorted penta-gonal-bipyramidal geometries with trans nitrosyl and chloride ligands. The title mol-ecule lies on a crystallographic inversion centre. The ethane group of the non-bridging depe ligand is positionally disordered, with site-occupancy factors of 0.63 and 0.37. In the crystal structure, the binuclear mol-ecules are linked by weak inter-molecular C-H⋯O and C-H⋯Cl inter-actions. In addition, weak intra-molecular C-H⋯Cl inter-actions are also present.

Entities:  

Year:  2008        PMID: 21201325      PMCID: PMC2960239          DOI: 10.1107/S1600536808001141

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


Related literature

For related literature, see: Avramović et al. (2008 ▶); Bencze & Kohàn (1982 ▶); Campbell et al. (1985 ▶); Carmona et al. (1989 ▶); Desiraju & Steiner (1999 ▶); Han & Coucouvanis (2002 ▶); Hunter & Legzdins (1984 ▶); Landau et al. (1999 ▶); Zeng et al. (1994 ▶).

Experimental

Crystal data

[W2Cl6(NO)2(C10H22P2)3] M = 1259.10 Orthorhombic, a = 12.6406 (14) Å b = 17.6485 (14) Å c = 20.5243 (17) Å V = 4578.7 (7) Å3 Z = 4 Mo Kα radiation μ = 5.61 mm−1 T = 183 (2) K 0.26 × 0.20 × 0.15 mm

Data collection

Stoe IPDS diffractometer Absorption correction: numerical (Coppens et al., 1965 ▶) T min = 0.329, T max = 0.499 52250 measured reflections 3982 independent reflections 3026 reflections with I > 2σ(I) R int = 0.079

Refinement

R[F 2 > 2σ(F 2)] = 0.024 wR(F 2) = 0.056 S = 0.84 3982 reflections 224 parameters 1 restraint H-atom parameters constrained Δρmax = 1.04 e Å−3 Δρmin = −1.27 e Å−3 Data collection: IPDS Software (Stoe & Cie, 1999 ▶); cell refinement: IPDS Software; data reduction: X-RED (Stoe & Cie, 1999 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶), SHELXL97 and PLATON (Spek, 2003 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808001141/su2041sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808001141/su2041Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[W2Cl6(NO)2(C10H22P2)3]F000 = 2488
Mr = 1259.10Dx = 1.827 Mg m3
Orthorhombic, PbcaMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 7997 reflections
a = 12.6406 (14) Åθ = 2.8–30.4º
b = 17.6485 (14) ŵ = 5.61 mm1
c = 20.5243 (17) ÅT = 183 (2) K
V = 4578.7 (7) Å3Block, yellow
Z = 40.26 × 0.20 × 0.15 mm
Stoe IPDS diffractometer3982 independent reflections
Radiation source: fine-focus sealed tube3026 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.079
T = 183(2) Kθmax = 25.0º
φ oscillation scanθmin = 2.8º
Absorption correction: numerical(Coppens et al., 1965)h = −15→15
Tmin = 0.329, Tmax = 0.499k = −20→20
52250 measured reflectionsl = −24→24
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.024H-atom parameters constrained
wR(F2) = 0.056  w = 1/[σ^2^(Fo^2^) + (0.0357P)^2^] where P = (Fo^2^ + 2Fc^2^)/3
S = 0.85(Δ/σ)max = 0.001
3982 reflectionsΔρmax = 1.04 e Å3
224 parametersΔρmin = −1.27 e Å3
1 restraintExtinction correction: none
Primary atom site location: structure-invariant direct methods
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 F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > σ(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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)
W10.826046 (13)0.388044 (11)0.379416 (7)0.01301 (6)
Cl10.77419 (9)0.50925 (7)0.43099 (5)0.0229 (3)
Cl20.95733 (9)0.33344 (8)0.30362 (5)0.0232 (3)
Cl30.76818 (10)0.45607 (8)0.27925 (5)0.0261 (3)
P10.75410 (11)0.26356 (8)0.33323 (6)0.0221 (3)
P20.62919 (11)0.38137 (9)0.40971 (8)0.0319 (3)
P30.99811 (9)0.46776 (7)0.39288 (5)0.0141 (3)
N10.8622 (3)0.3381 (2)0.45154 (17)0.0180 (9)
O10.8860 (3)0.3047 (2)0.50083 (16)0.0282 (9)
C10.6454 (7)0.2268 (5)0.3833 (5)0.0341 (16)0.631 (8)
H1A0.61410.18270.36270.041*0.631 (8)
H1B0.67160.21200.42590.041*0.631 (8)
C20.5642 (6)0.2887 (5)0.3901 (5)0.0341 (16)0.631 (8)
H2A0.51470.27560.42440.041*0.631 (8)
H2B0.52480.29340.34970.041*0.631 (8)
C30.6069 (13)0.2531 (10)0.3577 (7)0.0341 (16)0.369 (8)
H3A0.56190.28400.33010.041*0.369 (8)
H3B0.58420.20070.35470.041*0.369 (8)
C40.6042 (13)0.2805 (9)0.4274 (7)0.0341 (16)0.369 (8)
H4A0.65970.25800.45380.041*0.369 (8)
H4B0.53600.27230.44780.041*0.369 (8)
C50.8399 (6)0.1786 (4)0.3396 (3)0.0505 (18)
H5A0.79630.13450.33130.061*
H5B0.89170.18130.30480.061*
C60.8966 (6)0.1655 (4)0.4000 (4)0.072 (3)
H6A0.95300.20160.40400.107*
H6B0.92550.11520.39990.107*
H6C0.84890.17090.43610.107*
C70.7194 (6)0.2647 (3)0.2484 (3)0.0408 (15)
H7A0.67490.30850.24050.049*
H7B0.78370.27140.22320.049*
C80.6617 (5)0.1942 (4)0.2226 (3)0.0484 (18)
H8A0.70190.14970.23320.073*
H8B0.65420.19800.17620.073*
H8C0.59300.19090.24230.073*
C90.5410 (4)0.4353 (5)0.3574 (3)0.051 (2)
H9A0.55840.48860.36130.062*
H9B0.55350.42050.31260.062*
C100.4233 (5)0.4248 (7)0.3728 (3)0.099 (4)
H10A0.38170.44550.33800.148*
H10B0.40650.45040.41270.148*
H10C0.40800.37180.37730.148*
C110.5917 (5)0.4121 (4)0.4913 (3)0.0462 (19)
H11A0.59400.46700.49270.055*
H11B0.51920.39680.49920.055*
C120.6603 (6)0.3814 (6)0.5455 (3)0.082 (3)
H12A0.66580.32730.54150.123*
H12B0.62910.39380.58680.123*
H12C0.72950.40350.54280.123*
C131.0135 (4)0.5223 (3)0.46896 (19)0.0157 (10)
H13A1.08600.53980.47200.019*
H13B0.96820.56660.46680.019*
C141.1275 (4)0.4204 (3)0.3871 (2)0.0207 (10)
H14A1.13970.40680.34190.025*
H14B1.18180.45650.39940.025*
C151.1407 (4)0.3499 (3)0.4285 (3)0.0306 (13)
H15A1.13360.36300.47370.046*
H15B1.20940.32850.42110.046*
H15C1.08740.31350.41700.046*
C161.0053 (4)0.5396 (3)0.3298 (2)0.0239 (12)
H16A1.01120.51430.28800.029*
H16B0.93900.56740.32970.029*
C171.0947 (4)0.5963 (3)0.3352 (3)0.0340 (14)
H17A1.08750.62460.37490.051*
H17B1.09230.63050.29880.051*
H17C1.16120.57000.33520.051*
U11U22U33U12U13U23
W10.01297 (9)0.01534 (10)0.01072 (9)0.00073 (8)0.00014 (7)0.00121 (8)
Cl10.0221 (6)0.0214 (7)0.0251 (6)0.0079 (5)−0.0026 (5)−0.0062 (5)
Cl20.0198 (6)0.0291 (7)0.0206 (6)0.0006 (5)0.0059 (5)−0.0074 (5)
Cl30.0311 (7)0.0298 (8)0.0174 (5)0.0003 (6)−0.0063 (5)0.0073 (5)
P10.0230 (7)0.0242 (8)0.0190 (6)−0.0073 (6)0.0008 (5)−0.0066 (5)
P20.0183 (6)0.0265 (8)0.0510 (9)−0.0004 (7)0.0133 (6)−0.0013 (7)
P30.0145 (6)0.0166 (6)0.0113 (5)−0.0011 (5)0.0025 (4)0.0009 (4)
N10.0156 (19)0.025 (2)0.0137 (18)−0.0019 (18)−0.0001 (15)0.0010 (18)
O10.033 (2)0.028 (2)0.0232 (18)0.0046 (17)−0.0024 (16)0.0112 (16)
C10.022 (4)0.026 (4)0.055 (5)−0.006 (3)0.011 (3)0.000 (3)
C20.022 (4)0.026 (4)0.055 (5)−0.006 (3)0.011 (3)0.000 (3)
C30.022 (4)0.026 (4)0.055 (5)−0.006 (3)0.011 (3)0.000 (3)
C40.022 (4)0.026 (4)0.055 (5)−0.006 (3)0.011 (3)0.000 (3)
C50.073 (5)0.026 (4)0.052 (4)−0.012 (3)−0.027 (4)0.003 (3)
C60.068 (5)0.020 (4)0.127 (7)0.004 (4)−0.052 (5)0.004 (4)
C70.065 (4)0.026 (3)0.032 (3)−0.002 (3)−0.029 (3)−0.005 (3)
C80.063 (4)0.035 (4)0.047 (3)0.010 (3)−0.036 (3)−0.019 (3)
C90.023 (3)0.089 (6)0.042 (3)0.013 (3)−0.013 (3)−0.030 (4)
C100.015 (3)0.233 (13)0.049 (4)0.007 (5)−0.004 (3)−0.047 (6)
C110.026 (3)0.076 (6)0.037 (3)0.017 (3)0.017 (3)0.019 (3)
C120.045 (4)0.143 (9)0.058 (4)0.040 (5)0.025 (4)0.062 (5)
C130.019 (2)0.017 (3)0.011 (2)−0.006 (2)0.0019 (18)0.0006 (19)
C140.016 (2)0.022 (3)0.024 (2)0.002 (2)0.004 (2)−0.002 (2)
C150.028 (3)0.030 (3)0.034 (3)0.013 (2)−0.001 (2)0.000 (3)
C160.032 (3)0.024 (3)0.017 (2)−0.004 (2)0.004 (2)0.006 (2)
C170.034 (3)0.032 (4)0.036 (3)−0.008 (3)0.003 (2)0.017 (3)
W1—P12.5598 (13)C6—H6C0.9600
W1—P22.5675 (14)C7—C81.536 (8)
W1—P32.6051 (12)C7—H7A0.9700
W1—Cl12.4750 (12)C7—H7B0.9700
W1—Cl22.4703 (11)C8—H8A0.9600
W1—Cl32.4905 (11)C8—H8B0.9600
W1—N11.783 (4)C8—H8C0.9600
P1—C71.796 (5)C9—C101.531 (8)
P1—C11.834 (8)C9—H9A0.9700
P1—C51.855 (7)C9—H9B0.9700
P1—C31.936 (15)C10—H10A0.9600
P2—C91.817 (7)C10—H10B0.9600
P2—C111.822 (6)C10—H10C0.9600
P2—C41.844 (16)C11—C121.512 (8)
P2—C21.874 (9)C11—H11A0.9700
P3—C161.815 (5)C11—H11B0.9700
P3—C141.840 (5)C12—H12A0.9600
P3—C131.844 (4)C12—H12B0.9600
N1—O11.208 (5)C12—H12C0.9600
C1—C21.506 (10)C13—C13i1.535 (8)
C1—H1A0.9700C13—H13A0.9700
C1—H1B0.9700C13—H13B0.9700
C2—H2A0.9700C14—C151.516 (7)
C2—H2B0.9700C14—H14A0.9700
C3—C41.511 (10)C14—H14B0.9700
C3—H3A0.9700C15—H15A0.9600
C3—H3B0.9700C15—H15B0.9600
C4—H4A0.9700C15—H15C0.9600
C4—H4B0.9700C16—C171.514 (7)
C5—C61.450 (9)C16—H16A0.9700
C5—H5A0.9700C16—H16B0.9700
C5—H5B0.9700C17—H17A0.9600
C6—H6A0.9600C17—H17B0.9600
C6—H6B0.9600C17—H17C0.9600
N1—W1—Cl198.06 (14)P1—C5—H5B107.7
N1—W1—Cl299.08 (13)H5A—C5—H5B107.1
N1—W1—Cl3177.72 (13)C5—C6—H6A109.5
Cl1—W1—Cl2141.66 (4)C5—C6—H6B109.5
Cl2—W1—Cl382.27 (4)H6A—C6—H6B109.5
Cl1—W1—Cl381.87 (4)C5—C6—H6C109.5
N1—W1—P188.51 (14)H6A—C6—H6C109.5
Cl1—W1—P1143.71 (4)H6B—C6—H6C109.5
Cl1—W1—P271.30 (5)C8—C7—P1116.2 (4)
Cl1—W1—P373.09 (4)C8—C7—H7A108.2
Cl2—W1—P170.77 (4)P1—C7—H7A108.2
Cl2—W1—P373.54 (4)C8—C7—H7B108.2
Cl3—W1—P190.21 (4)P1—C7—H7B108.2
N1—W1—P291.41 (13)H7A—C7—H7B107.4
Cl2—W1—P2141.78 (5)C7—C8—H8A109.5
Cl3—W1—P286.41 (5)C7—C8—H8B109.5
P1—W1—P272.90 (5)H8A—C8—H8B109.5
N1—W1—P388.00 (13)C7—C8—H8C109.5
Cl3—W1—P394.16 (4)H8A—C8—H8C109.5
P1—W1—P3143.07 (4)H8B—C8—H8C109.5
P2—W1—P3143.92 (4)C10—C9—P2114.3 (6)
C7—P1—C1111.4 (4)C10—C9—H9A108.7
C7—P1—C5102.7 (3)P2—C9—H9A108.7
C1—P1—C596.5 (4)C10—C9—H9B108.7
C7—P1—C391.0 (5)P2—C9—H9B108.7
C5—P1—C3117.8 (6)H9A—C9—H9B107.6
C7—P1—W1115.9 (2)C9—C10—H10A109.5
C1—P1—W1111.2 (3)C9—C10—H10B109.5
C5—P1—W1117.3 (2)H10A—C10—H10B109.5
C3—P1—W1109.1 (5)C9—C10—H10C109.5
C9—P2—C11103.1 (3)H10A—C10—H10C109.5
C9—P2—C4121.1 (6)H10B—C10—H10C109.5
C11—P2—C493.5 (5)C12—C11—P2114.9 (5)
C9—P2—C293.5 (4)C12—C11—H11A108.5
C11—P2—C2110.1 (4)P2—C11—H11A108.5
C9—P2—W1115.3 (2)C12—C11—H11B108.5
C11—P2—W1117.4 (2)P2—C11—H11B108.5
C4—P2—W1104.9 (5)H11A—C11—H11B107.5
C2—P2—W1114.4 (3)C11—C12—H12A109.5
C16—P3—C14103.1 (2)C11—C12—H12B109.5
C16—P3—C13103.6 (2)H12A—C12—H12B109.5
C14—P3—C13101.4 (2)C11—C12—H12C109.5
C16—P3—W1110.08 (17)H12A—C12—H12C109.5
C14—P3—W1119.35 (17)H12B—C12—H12C109.5
C13—P3—W1117.34 (15)C13i—C13—P3114.4 (4)
O1—N1—W1179.3 (4)C13i—C13—H13A108.7
C2—C1—P1107.8 (7)P3—C13—H13A108.7
C2—C1—H1A110.1C13i—C13—H13B108.7
P1—C1—H1A110.1P3—C13—H13B108.7
C2—C1—H1B110.1H13A—C13—H13B107.6
P1—C1—H1B110.1C15—C14—P3115.7 (3)
H1A—C1—H1B108.5C15—C14—H14A108.3
C1—C2—P2110.7 (6)P3—C14—H14A108.3
C1—C2—H2A109.5C15—C14—H14B108.3
P2—C2—H2A109.5P3—C14—H14B108.3
C1—C2—H2B109.5H14A—C14—H14B107.4
P2—C2—H2B109.5C14—C15—H15A109.5
H2A—C2—H2B108.1C14—C15—H15B109.5
C4—C3—P1103.7 (10)H15A—C15—H15B109.5
C4—C3—H3A111.0C14—C15—H15C109.5
P1—C3—H3A111.0H15A—C15—H15C109.5
C4—C3—H3B111.0H15B—C15—H15C109.5
P1—C3—H3B111.0C17—C16—P3116.6 (4)
H3A—C3—H3B109.0C17—C16—H16A108.2
C3—C4—P296.8 (11)P3—C16—H16A108.2
C3—C4—H4A112.4C17—C16—H16B108.2
P2—C4—H4A112.4P3—C16—H16B108.2
C3—C4—H4B112.4H16A—C16—H16B107.3
P2—C4—H4B112.4C16—C17—H17A109.5
H4A—C4—H4B110.0C16—C17—H17B109.5
C6—C5—P1118.6 (5)H17A—C17—H17B109.5
C6—C5—H5A107.7C16—C17—H17C109.5
P1—C5—H5A107.7H17A—C17—H17C109.5
C6—C5—H5B107.7H17B—C17—H17C109.5
N1—W1—P1—C7−169.6 (3)Cl2—W1—P3—C14−36.06 (18)
Cl2—W1—P1—C7−69.4 (3)Cl1—W1—P3—C14163.07 (18)
Cl1—W1—P1—C788.8 (3)Cl3—W1—P3—C14−116.74 (18)
Cl3—W1—P1—C712.3 (3)P1—W1—P3—C14−20.84 (19)
P2—W1—P1—C798.5 (3)P2—W1—P3—C14153.66 (18)
P3—W1—P1—C7−84.9 (3)N1—W1—P3—C13−59.1 (2)
N1—W1—P1—C161.9 (4)Cl2—W1—P3—C13−159.16 (18)
Cl2—W1—P1—C1162.1 (4)Cl1—W1—P3—C1339.97 (17)
Cl1—W1—P1—C1−39.7 (4)Cl3—W1—P3—C13120.16 (18)
Cl3—W1—P1—C1−116.2 (4)P1—W1—P3—C13−143.94 (18)
P2—W1—P1—C1−30.0 (4)P2—W1—P3—C1330.6 (2)
P3—W1—P1—C1146.6 (4)C7—P1—C1—C2−77.2 (8)
N1—W1—P1—C5−47.8 (3)C5—P1—C1—C2176.4 (7)
Cl2—W1—P1—C552.4 (3)C3—P1—C1—C2−36.6 (10)
Cl1—W1—P1—C5−149.4 (3)W1—P1—C1—C253.7 (8)
Cl3—W1—P1—C5134.1 (3)P1—C1—C2—P2−45.4 (9)
P2—W1—P1—C5−139.7 (3)C9—P2—C2—C1140.7 (8)
P3—W1—P1—C536.9 (3)C11—P2—C2—C1−113.9 (7)
N1—W1—P1—C389.5 (5)C4—P2—C2—C1−55.6 (10)
Cl2—W1—P1—C3−170.3 (5)W1—P2—C2—C120.8 (9)
Cl1—W1—P1—C3−12.1 (5)C7—P1—C3—C4−158.7 (11)
Cl3—W1—P1—C3−88.6 (5)C1—P1—C3—C458.6 (11)
P2—W1—P1—C3−2.4 (5)C5—P1—C3—C496.3 (12)
P3—W1—P1—C3174.2 (5)W1—P1—C3—C4−40.8 (13)
N1—W1—P2—C9172.8 (3)P1—C3—C4—P269.6 (11)
Cl2—W1—P2—C9−80.6 (3)C9—P2—C4—C358.9 (12)
Cl1—W1—P2—C974.7 (3)C11—P2—C4—C3166.5 (10)
Cl3—W1—P2—C9−7.9 (3)C2—P2—C4—C339.8 (8)
P1—W1—P2—C9−99.2 (3)W1—P2—C4—C3−73.8 (11)
P3—W1—P2—C984.2 (3)C7—P1—C5—C6170.9 (6)
N1—W1—P2—C1150.8 (3)C1—P1—C5—C6−75.4 (7)
Cl2—W1—P2—C11157.5 (3)C3—P1—C5—C6−91.1 (8)
Cl1—W1—P2—C11−47.2 (3)W1—P1—C5—C642.5 (7)
Cl3—W1—P2—C11−129.8 (3)C1—P1—C7—C8−43.2 (6)
P1—W1—P2—C11138.8 (3)C5—P1—C7—C859.1 (6)
P3—W1—P2—C11−37.7 (3)C3—P1—C7—C8−59.7 (7)
N1—W1—P2—C4−51.3 (5)W1—P1—C7—C8−171.6 (4)
Cl2—W1—P2—C455.3 (5)C11—P2—C9—C10−55.8 (6)
Cl1—W1—P2—C4−149.4 (5)C4—P2—C9—C1046.6 (8)
Cl3—W1—P2—C4128.0 (5)C2—P2—C9—C1055.7 (6)
P1—W1—P2—C436.7 (5)W1—P2—C9—C10174.8 (5)
P3—W1—P2—C4−139.9 (5)C9—P2—C11—C12−174.5 (6)
N1—W1—P2—C2−80.5 (4)C4—P2—C11—C1262.4 (8)
Cl2—W1—P2—C226.2 (4)C2—P2—C11—C1286.8 (7)
Cl1—W1—P2—C2−178.5 (4)W1—P2—C11—C12−46.4 (7)
Cl3—W1—P2—C298.9 (4)C16—P3—C13—C13i167.4 (5)
P1—W1—P2—C27.5 (4)C14—P3—C13—C13i−85.9 (5)
P3—W1—P2—C2−169.0 (4)W1—P3—C13—C13i45.9 (5)
N1—W1—P3—C16−177.1 (2)C16—P3—C14—C15−172.3 (4)
Cl2—W1—P3—C1682.81 (18)C13—P3—C14—C1580.6 (4)
Cl1—W1—P3—C16−78.06 (18)W1—P3—C14—C15−50.0 (4)
Cl3—W1—P3—C162.13 (18)C14—P3—C16—C17−58.1 (5)
P1—W1—P3—C1698.03 (19)C13—P3—C16—C1747.3 (5)
P2—W1—P3—C16−87.5 (2)W1—P3—C16—C17173.5 (4)
N1—W1—P3—C1464.0 (2)
D—H···AD—HH···AD···AD—H···A
C5—H5B···Cl20.972.813.196 (7)105
C11—H11A···Cl10.972.713.129 (7)107
C13—H13B···Cl10.972.753.132 (5)104
C14—H14A···Cl20.972.763.150 (5)105
C13—H13A···Cl1i0.972.803.425 (5)123
C10—H10A···Cl3ii0.962.813.726 (7)161
C2—H2A···O1iii0.972.653.579 (10)161
C4—H4B···O1iii0.972.563.470 (15)156
W1—P12.5598 (13)
W1—P22.5675 (14)
W1—P32.6051 (12)
W1—Cl12.4750 (12)
W1—Cl22.4703 (11)
W1—Cl32.4905 (11)
W1—N11.783 (4)
N1—W1—Cl198.06 (14)
N1—W1—Cl299.08 (13)
N1—W1—Cl3177.72 (13)
Cl1—W1—Cl2141.66 (4)
Cl2—W1—Cl382.27 (4)
Cl1—W1—Cl381.87 (4)
Cl1—W1—P271.30 (5)
Cl1—W1—P373.09 (4)
Cl2—W1—P170.77 (4)
Cl2—W1—P373.54 (4)
Cl3—W1—P190.21 (4)
P1—W1—P272.90 (5)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
C5—H5B⋯Cl20.972.813.196 (7)105
C11—H11A⋯Cl10.972.713.129 (7)107
C13—H13B⋯Cl10.972.753.132 (5)104
C14—H14A⋯Cl20.972.763.150 (5)105
C13—H13A⋯Cl1i0.972.803.425 (5)123
C10—H10A⋯Cl3ii0.962.813.726 (7)161
C2—H2A⋯O1iii0.972.653.579 (10)161
C4—H4B⋯O1iii0.972.563.470 (15)156

Symmetry codes: (i) ; (ii) ; (iii) .

  4 in total

1.  A short history of SHELX.

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

2.  Synthesis and structure of singly bridged and doubly bridged [MoFe(3)S(4)] double cubanes with bidentate phosphine ligands.

Authors:  Jaehong Han; Dimitri Coucouvanis
Journal:  Inorg Chem       Date:  2002-05-20       Impact factor: 5.165

3.  Acidic Dicationic Iron(II) Dihydrogen Complexes and Compounds Related by H(2) Substitution.

Authors:  Shaun E. Landau; Robert H. Morris; Alan J. Lough
Journal:  Inorg Chem       Date:  1999-12-27       Impact factor: 5.165

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

Authors:  Nataša Avramović; Olivier Blacque; Helmut W Schmalle; Heinz Berke
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2007-12-22
  4 in total

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