Crystal structure of (OC)₅W(μ-dppe)W(CO)₅

In the title complex two W(CO)₅ moieties are bridged by a bis­(di­phenyl­phosphan­yl)ethane (dppe) ligand. Both tungsten atoms have a slightly distorted octa­hedral coordination.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.021
• wR factor = 0.048
• Data-to-parameter ratio = 14.4

checkCIF/PLATON results

No syntax errors found



Alert level G
PLAT230_ALERT_2_G Hirshfeld Test Diff for    O2     --  C15     ..        5.5 s.u.
PLAT230_ALERT_2_G Hirshfeld Test Diff for    O5     --  C18     ..        6.5 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  W1     --  C14     ..        5.9 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  W1     --  C15     ..        7.3 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  W1     --  C16     ..        5.9 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  W1     --  C18     ..        7.4 s.u.
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density           8 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   0 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   7 ALERT level G = General information/check it is not something unexpected

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   7 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: APEX2 (Bruker, 2011); cell refinement: SAINT (Bruker, 2011); data reduction: SAINT (Bruker, 2011); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: X-SEED (Barbour, 2001).

[µ-Ethane-1,2-diylbis(diphenylphosphane)-κ²P:P']bis[pentacarbonyltungsten(0)]

Crystal data

[W2(C26H24P2)(CO)10]	F(000) = 996
Mr = 1046.17	Dx = 1.958 Mg m^−3
Monoclinic, P21/n	Cu Kα radiation, λ = 1.54178 Å
a = 9.8193 (4) Å	Cell parameters from 8094 reflections
b = 16.0492 (7) Å	θ = 4.6–66.6°
c = 11.3312 (5) Å	µ = 13.15 mm^−1
β = 96.511 (2)°	T = 100 K
V = 1774.19 (13) Å^3	Transparent rhomboid, colorless
Z = 2	0.15 × 0.14 × 0.06 mm

Data collection

Bruker APEXII CCD diffractometer	2954 reflections with I > 2σ(I)
Detector resolution: 8.33 pixels mm^-1	Rint = 0.056
phi and ω scans	θmax = 68.2°, θmin = 4.8°
Absorption correction: multi-scan (SADABS; Bruker, 2011)	h = −11→11
Tmin = 0.254, Tmax = 0.756	k = −19→19
26419 measured reflections	l = −13→13
3256 independent reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.021	H-atom parameters constrained
wR(F^2) = 0.048	w = 1/[σ^2(Fo^2) + (0.0218P)^2 + 0.5664P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = 0.001
3256 reflections	Δρmax = 0.54 e Å^−3
226 parameters	Δρmin = −0.58 e Å^−3

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. All nonhydrogen atoms were located in a single difference Fourier electron density maps and refined using anisotropic diplacement parameters. All C-H hydrogen atoms were placed in calculated positions with Uiso = 1.2xUeqiv of the connected C atoms

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
W1	0.17092 (2)	0.47944 (2)	0.81902 (2)	0.01462 (6)
P1	0.15114 (8)	0.56563 (5)	0.63197 (7)	0.01359 (16)
O1	0.1345 (2)	0.64362 (16)	0.9701 (2)	0.0277 (6)
O2	−0.1519 (2)	0.44991 (18)	0.7958 (2)	0.0324 (6)
O3	0.2025 (2)	0.36975 (16)	1.0520 (2)	0.0286 (6)
O4	0.2103 (3)	0.31759 (16)	0.6641 (2)	0.0317 (6)
O5	0.4947 (2)	0.50864 (15)	0.8560 (2)	0.0274 (6)
C1	0.0518 (3)	0.66234 (19)	0.6298 (3)	0.0162 (6)
C2	0.0733 (3)	0.7262 (2)	0.5503 (3)	0.0206 (7)
H2	0.1383	0.7188	0.4950	0.025*
C3	0.0010 (3)	0.8002 (2)	0.5510 (3)	0.0251 (8)
H3	0.0155	0.8429	0.4958	0.030*
C4	−0.0924 (3)	0.8119 (2)	0.6323 (3)	0.0253 (8)
H4	−0.1402	0.8633	0.6342	0.030*
C5	−0.1164 (3)	0.7490 (2)	0.7106 (3)	0.0238 (7)
H5	−0.1813	0.7571	0.7657	0.029*
C6	−0.0453 (3)	0.6737 (2)	0.7089 (3)	0.0196 (7)
H6	−0.0633	0.6301	0.7618	0.023*
C7	0.3146 (3)	0.60406 (19)	0.5907 (3)	0.0149 (6)
C8	0.3683 (3)	0.5823 (2)	0.4868 (3)	0.0202 (7)
H8	0.3191	0.5455	0.4319	0.024*
C9	0.4940 (3)	0.6143 (2)	0.4630 (3)	0.0264 (8)
H9	0.5300	0.5991	0.3917	0.032*
C10	0.5671 (3)	0.6679 (2)	0.5420 (3)	0.0260 (8)
H10	0.6532	0.6892	0.5256	0.031*
C11	0.5130 (4)	0.6903 (2)	0.6460 (3)	0.0269 (8)
H11	0.5614	0.7280	0.7001	0.032*
C12	0.3894 (3)	0.6578 (2)	0.6706 (3)	0.0218 (7)
H12	0.3546	0.6722	0.7428	0.026*
C13	0.0738 (3)	0.51389 (19)	0.4953 (3)	0.0146 (6)
H13A	0.0747	0.5528	0.4275	0.018*
H13B	0.1297	0.4647	0.4793	0.018*
C14	0.1472 (3)	0.5850 (2)	0.9158 (3)	0.0205 (7)
C15	−0.0363 (4)	0.4607 (2)	0.8030 (3)	0.0213 (7)
C16	0.1906 (3)	0.4096 (2)	0.9678 (3)	0.0207 (7)
C17	0.1959 (3)	0.3754 (2)	0.7191 (3)	0.0202 (7)
C18	0.3793 (4)	0.4984 (2)	0.8413 (3)	0.0205 (7)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
W1	0.01547 (9)	0.01626 (9)	0.01235 (9)	−0.00103 (5)	0.00255 (5)	0.00059 (6)
P1	0.0139 (4)	0.0142 (4)	0.0128 (4)	−0.0021 (3)	0.0019 (3)	−0.0009 (3)
O1	0.0315 (14)	0.0288 (14)	0.0221 (13)	0.0051 (11)	−0.0009 (10)	−0.0088 (12)
O2	0.0196 (14)	0.0540 (18)	0.0243 (13)	−0.0101 (12)	0.0050 (10)	0.0027 (13)
O3	0.0304 (14)	0.0356 (15)	0.0209 (13)	0.0049 (11)	0.0071 (10)	0.0106 (12)
O4	0.0430 (16)	0.0231 (14)	0.0311 (14)	−0.0061 (11)	0.0128 (12)	−0.0054 (12)
O5	0.0162 (13)	0.0269 (13)	0.0380 (15)	−0.0008 (10)	−0.0017 (10)	0.0032 (12)
C1	0.0159 (15)	0.0160 (15)	0.0157 (16)	−0.0016 (12)	−0.0030 (12)	−0.0033 (13)
C2	0.0194 (16)	0.0193 (17)	0.0230 (17)	0.0002 (13)	0.0012 (13)	−0.0001 (15)
C3	0.0227 (17)	0.0193 (17)	0.0319 (19)	−0.0013 (14)	−0.0028 (14)	0.0053 (16)
C4	0.0167 (16)	0.0219 (17)	0.035 (2)	0.0033 (14)	−0.0070 (14)	−0.0069 (16)
C5	0.0157 (16)	0.0307 (19)	0.0244 (18)	0.0028 (14)	0.0003 (13)	−0.0076 (16)
C6	0.0157 (15)	0.0255 (18)	0.0170 (16)	0.0007 (13)	0.0001 (13)	−0.0011 (14)
C7	0.0159 (15)	0.0133 (15)	0.0158 (15)	−0.0010 (12)	0.0029 (12)	0.0043 (13)
C8	0.0186 (16)	0.0198 (17)	0.0224 (17)	−0.0024 (13)	0.0027 (13)	0.0000 (14)
C9	0.0210 (17)	0.033 (2)	0.0259 (18)	0.0012 (15)	0.0080 (14)	0.0037 (17)
C10	0.0179 (17)	0.0234 (18)	0.037 (2)	−0.0029 (14)	0.0057 (15)	0.0068 (17)
C11	0.0228 (18)	0.0254 (18)	0.032 (2)	−0.0090 (14)	0.0025 (15)	−0.0033 (17)
C12	0.0184 (16)	0.0236 (18)	0.0243 (18)	−0.0023 (14)	0.0063 (13)	−0.0030 (15)
C13	0.0177 (16)	0.0152 (15)	0.0109 (15)	−0.0028 (12)	0.0007 (12)	−0.0027 (13)
C14	0.0175 (16)	0.0303 (19)	0.0136 (16)	0.0017 (13)	0.0016 (13)	0.0012 (15)
C15	0.029 (2)	0.0228 (18)	0.0132 (16)	−0.0016 (14)	0.0055 (13)	0.0010 (14)
C16	0.0192 (16)	0.0230 (17)	0.0209 (18)	0.0021 (13)	0.0062 (13)	−0.0015 (16)
C17	0.0241 (17)	0.0188 (17)	0.0186 (17)	−0.0033 (13)	0.0067 (13)	0.0024 (15)
C18	0.029 (2)	0.0147 (16)	0.0180 (17)	−0.0001 (14)	0.0025 (14)	0.0002 (14)

Geometric parameters (Å, º)

W1—C16	2.015 (3)	C4—C5	1.381 (5)
W1—C15	2.044 (4)	C4—H4	0.9500
W1—C14	2.045 (4)	C5—C6	1.398 (5)
W1—C17	2.048 (3)	C5—H5	0.9500
W1—C18	2.056 (4)	C6—H6	0.9500
W1—P1	2.5200 (8)	C7—C8	1.388 (4)
P1—C7	1.829 (3)	C7—C12	1.397 (5)
P1—C1	1.832 (3)	C8—C9	1.391 (5)
P1—C13	1.843 (3)	C8—H8	0.9500
O1—C14	1.140 (4)	C9—C10	1.382 (5)
O2—C15	1.143 (4)	C9—H9	0.9500
O3—C16	1.144 (4)	C10—C11	1.394 (5)
O4—C17	1.135 (4)	C10—H10	0.9500
O5—C18	1.139 (4)	C11—C12	1.378 (5)
C1—C6	1.393 (4)	C11—H11	0.9500
C1—C2	1.397 (5)	C12—H12	0.9500
C2—C3	1.384 (5)	C13—C13^i	1.531 (6)
C2—H2	0.9500	C13—H13A	0.9900
C3—C4	1.385 (5)	C13—H13B	0.9900
C3—H3	0.9500
C16—W1—C15	89.55 (13)	C4—C5—H5	119.9
C16—W1—C14	91.03 (13)	C6—C5—H5	119.9
C15—W1—C14	89.83 (13)	C1—C6—C5	120.1 (3)
C16—W1—C17	90.16 (13)	C1—C6—H6	120.0
C15—W1—C17	90.64 (13)	C5—C6—H6	120.0
C14—W1—C17	178.72 (13)	C8—C7—C12	118.8 (3)
C16—W1—C18	88.85 (13)	C8—C7—P1	124.1 (2)
C15—W1—C18	178.03 (12)	C12—C7—P1	117.0 (2)
C14—W1—C18	89.05 (13)	C7—C8—C9	120.2 (3)
C17—W1—C18	90.52 (13)	C7—C8—H8	119.9
C16—W1—P1	178.79 (9)	C9—C8—H8	119.9
C15—W1—P1	91.45 (9)	C10—C9—C8	120.7 (3)
C14—W1—P1	89.64 (9)	C10—C9—H9	119.6
C17—W1—P1	89.16 (9)	C8—C9—H9	119.6
C18—W1—P1	90.16 (9)	C9—C10—C11	119.2 (3)
C7—P1—C1	101.08 (14)	C9—C10—H10	120.4
C7—P1—C13	103.13 (14)	C11—C10—H10	120.4
C1—P1—C13	101.69 (14)	C12—C11—C10	120.2 (3)
C7—P1—W1	114.44 (10)	C12—C11—H11	119.9
C1—P1—W1	117.80 (11)	C10—C11—H11	119.9
C13—P1—W1	116.38 (10)	C11—C12—C7	120.8 (3)
C6—C1—C2	118.9 (3)	C11—C12—H12	119.6
C6—C1—P1	120.3 (2)	C7—C12—H12	119.6
C2—C1—P1	120.7 (2)	C13^i—C13—P1	112.1 (3)
C3—C2—C1	120.7 (3)	C13^i—C13—H13A	109.2
C3—C2—H2	119.6	P1—C13—H13A	109.2
C1—C2—H2	119.6	C13^i—C13—H13B	109.2
C2—C3—C4	120.0 (3)	P1—C13—H13B	109.2
C2—C3—H3	120.0	H13A—C13—H13B	107.9
C4—C3—H3	120.0	O1—C14—W1	179.7 (3)
C5—C4—C3	120.1 (3)	O2—C15—W1	179.0 (3)
C5—C4—H4	119.9	O3—C16—W1	179.6 (3)
C3—C4—H4	119.9	O4—C17—W1	179.6 (3)
C4—C5—C6	120.2 (3)	O5—C18—W1	178.7 (3)
C7—P1—C1—C6	−146.7 (3)	W1—P1—C7—C8	117.1 (3)
C13—P1—C1—C6	107.2 (3)	C1—P1—C7—C12	65.5 (3)
W1—P1—C1—C6	−21.3 (3)	C13—P1—C7—C12	170.5 (3)
C7—P1—C1—C2	32.5 (3)	W1—P1—C7—C12	−62.2 (3)
C13—P1—C1—C2	−73.6 (3)	C12—C7—C8—C9	−0.5 (5)
W1—P1—C1—C2	157.9 (2)	P1—C7—C8—C9	−179.7 (3)
C6—C1—C2—C3	1.0 (5)	C7—C8—C9—C10	0.0 (5)
P1—C1—C2—C3	−178.1 (3)	C8—C9—C10—C11	−0.5 (5)
C1—C2—C3—C4	0.9 (5)	C9—C10—C11—C12	1.4 (5)
C2—C3—C4—C5	−1.7 (5)	C10—C11—C12—C7	−1.8 (5)
C3—C4—C5—C6	0.7 (5)	C8—C7—C12—C11	1.4 (5)
C2—C1—C6—C5	−2.1 (5)	P1—C7—C12—C11	−179.4 (3)
P1—C1—C6—C5	177.1 (2)	C7—P1—C13—C13^i	−172.8 (3)
C4—C5—C6—C1	1.2 (5)	C1—P1—C13—C13^i	−68.3 (3)
C1—P1—C7—C8	−115.3 (3)	W1—P1—C13—C13^i	61.0 (3)
C13—P1—C7—C8	−10.3 (3)

Symmetry code: (i) −x, −y+1, −z+1.