Bis(μ-di­phenyl­phosphido)­bis{trans-tri­carbonyl­bis­[1-(4-ethoxy­butoxy)­pentyl­idene]­rhenium}

The geometric centre of the title mol­ecule, Re₂(μ-PPh₂)₂(CO)₆[ax-C(ⁿBu)(OBuOEt)]₂ or [Re₂(C₁₁H₂₂O₂)₂(C₁₂H₁₀P)₂(CO)₆], lies on a crystallographic inversion centre, realising a trans-position of the two Z-configurated carbene ligands.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.009 Å
• R factor = 0.028
• wR factor = 0.066
• Data-to-parameter ratio = 18.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



ABSTM_02  Alert C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
          Tmin and Tmax reported:      0.150     0.409
          Tmin and Tmax expected:      0.111     0.387
          RR =      1.274
          Please check that your absorption correction is appropriate.

REFLT_03
         From the CIF: _diffrn_reflns_theta_max           27.56
         From the CIF: _reflns_number_total               5615
         TEST2: Reflns within _diffrn_reflns_theta_max
         Count of symmetry unique reflns         6028
         Completeness (_total/calc)             93.15%
          Alert C: < 95% complete

General Notes



ABSTM_02  When printed, the submitted absorption T values will be replaced
          by the scaled T values. Since the ratio of scaled T's is
          identical to the ratio of reported T values, the scaling does
          not imply a change to the absorption corrections used in the
          study.
          Ratio of Tmax expected/reported      0.946
          Tmax scaled      0.387 Tmin scaled      0.142


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 2 Alert Level C = Please check

---

Computing details

Data collection: XSCANS (Bruker, 1996); cell refinement: XSCANS; data reduction: SHELXTL (Bruker, 1998); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Bis(µ-diphenylphosphido)bis{trans-tricarbonylbis[1-(4- ethoxybutoxy)pentylidene]rhenium}

Crystal data

[Re2(C11H22O2)2(C12H10P)2(CO)6]	Z = 1
Mr = 1283.37	F(000) = 636
Triclinic, P1	Dx = 1.633 Mg m^−3
a = 10.294 (6) Å	Mo Kα radiation, λ = 0.71073 Å
b = 12.102 (5) Å	Cell parameters from 25 reflections
c = 12.230 (6) Å	θ = 8–15°
α = 69.86 (2)°	µ = 4.75 mm^−1
β = 86.58 (2)°	T = 293 K
γ = 66.39 (2)°	Prism, yellow
V = 1305.3 (11) Å^3	0.49 × 0.41 × 0.20 mm

Data collection

Bruker P4 diffractometer	4907 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.026
Graphite monochromator	θmax = 27.6°, θmin = 2.6°
ω scans	h = −13→13
Absorption correction: ψ scan (North et al., 1968)	k = −14→15
Tmin = 0.150, Tmax = 0.409	l = 0→15
5891 measured reflections	2 standard reflections every 400 reflections
5615 independent reflections	intensity decay: <1%

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.028	H-atom parameters constrained
wR(F^2) = 0.066	w = 1/[σ^2(Fo^2) + (0.0371P)^2 + 0.5044P] where P = (Fo^2 + 2Fc^2)/3
S = 1.04	(Δ/σ)max = 0.001
5615 reflections	Δρmax = 1.00 e Å^−3
299 parameters	Δρmin = −0.87 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0081 (4)

Special details

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.

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

	x	y	z	Uiso*/Ueq
Re1	1.125433 (15)	0.055541 (15)	0.381509 (13)	0.04152 (7)
P1	0.99320 (10)	−0.09052 (10)	0.43864 (8)	0.0401 (2)
C1	1.2072 (5)	0.0222 (4)	0.2442 (4)	0.0561 (10)
O1	1.2602 (4)	0.0074 (4)	0.1614 (3)	0.0853 (11)
C2	1.2184 (5)	0.1713 (5)	0.3601 (4)	0.0600 (11)
O2	1.2764 (5)	0.2377 (4)	0.3453 (4)	0.0929 (13)
C3	1.2991 (5)	−0.0869 (5)	0.4764 (4)	0.0565 (10)
O3	1.4052 (4)	−0.1641 (4)	0.5222 (4)	0.0861 (12)
C11	1.1079 (4)	−0.2625 (4)	0.4633 (4)	0.0470 (9)
C12	1.2311 (5)	−0.2983 (5)	0.4089 (5)	0.0694 (13)
H12	1.2601	−0.2356	0.3606	0.083*
C13	1.3125 (7)	−0.4273 (6)	0.4257 (6)	0.0884 (18)
H13	1.3957	−0.4494	0.3886	0.106*
C14	1.2741 (6)	−0.5208 (5)	0.4943 (6)	0.0816 (16)
H14	1.3296	−0.6067	0.5045	0.098*
C15	1.1522 (7)	−0.4875 (5)	0.5486 (6)	0.0854 (17)
H15	1.1243	−0.5511	0.5967	0.102*
C16	1.0698 (6)	−0.3594 (5)	0.5326 (5)	0.0711 (13)
H16	0.9864	−0.3383	0.5697	0.085*
C21	0.8686 (4)	−0.0639 (4)	0.3195 (3)	0.0454 (9)
C22	0.7432 (5)	−0.0799 (5)	0.3417 (5)	0.0659 (12)
H22	0.7176	−0.1022	0.4179	0.079*
C23	0.6548 (7)	−0.0626 (6)	0.2496 (6)	0.0857 (18)
H23	0.5697	−0.0725	0.2651	0.103*
C24	0.6906 (7)	−0.0316 (5)	0.1374 (5)	0.0813 (17)
H24	0.6312	−0.0211	0.0768	0.098*
C25	0.8139 (7)	−0.0164 (5)	0.1156 (5)	0.0789 (16)
H25	0.8391	0.0051	0.0392	0.095*
C26	0.9033 (5)	−0.0326 (4)	0.2051 (4)	0.0596 (11)
H26	0.9878	−0.0222	0.1881	0.071*
C4	0.9463 (4)	0.2108 (4)	0.2761 (4)	0.0459 (9)
O4	0.8191 (3)	0.2241 (3)	0.3075 (2)	0.0495 (6)
C31	0.6835 (4)	0.3317 (4)	0.2490 (4)	0.0570 (10)
H31A	0.7021	0.4002	0.1903	0.068*
H31B	0.6278	0.3658	0.3057	0.068*
C32	0.6024 (5)	0.2832 (4)	0.1925 (4)	0.0562 (11)
H32A	0.6022	0.2035	0.2477	0.067*
H32B	0.6494	0.2654	0.1256	0.067*
C33	0.4500 (5)	0.3813 (4)	0.1530 (4)	0.0586 (11)
H33A	0.3992	0.3906	0.2208	0.070*
H33B	0.4499	0.4643	0.1060	0.070*
C34	0.3754 (5)	0.3400 (5)	0.0824 (5)	0.0696 (13)
H34A	0.3903	0.2509	0.1228	0.084*
H34B	0.2739	0.3927	0.0718	0.084*
O5	0.4311 (5)	0.3543 (4)	−0.0259 (3)	0.0843 (11)
C36	0.4003 (8)	0.2918 (7)	−0.0906 (6)	0.0954 (19)
H36A	0.2989	0.3314	−0.1142	0.114*
H36B	0.4253	0.2023	−0.0426	0.114*
C37	0.4792 (10)	0.2991 (8)	−0.1940 (8)	0.124 (3)
H37A	0.4573	0.2551	−0.2374	0.187*
H37B	0.5794	0.2594	−0.1704	0.187*
H37C	0.4528	0.3877	−0.2422	0.187*
C38	0.9572 (5)	0.3110 (5)	0.1647 (4)	0.0604 (11)
H38A	1.0543	0.3045	0.1631	0.073*
H38B	0.8961	0.3959	0.1658	0.073*
C39	0.9159 (6)	0.2981 (5)	0.0533 (4)	0.0728 (14)
H39A	0.9441	0.2076	0.0660	0.087*
H39B	0.8132	0.3405	0.0369	0.087*
C40	0.9831 (7)	0.3548 (7)	−0.0508 (5)	0.0912 (18)
H40A	1.0854	0.3056	−0.0379	0.109*
H40B	0.9645	0.4422	−0.0576	0.109*
C41	0.9306 (8)	0.3570 (7)	−0.1642 (6)	0.113 (3)
H41A	0.9788	0.3931	−0.2268	0.170*
H41B	0.8299	0.4084	−0.1795	0.170*
H41C	0.9494	0.2707	−0.1587	0.170*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Re1	0.04409 (10)	0.05105 (11)	0.03233 (9)	−0.02332 (7)	0.00368 (5)	−0.01321 (6)
P1	0.0453 (5)	0.0453 (5)	0.0328 (5)	−0.0203 (4)	0.0012 (4)	−0.0144 (4)
C1	0.054 (2)	0.063 (3)	0.043 (2)	−0.019 (2)	0.0047 (19)	−0.015 (2)
O1	0.087 (3)	0.112 (3)	0.051 (2)	−0.029 (2)	0.0243 (18)	−0.037 (2)
C2	0.063 (3)	0.081 (3)	0.048 (2)	−0.043 (2)	0.008 (2)	−0.021 (2)
O2	0.107 (3)	0.120 (3)	0.085 (3)	−0.089 (3)	0.015 (2)	−0.026 (3)
C3	0.051 (2)	0.069 (3)	0.044 (2)	−0.025 (2)	0.0047 (19)	−0.012 (2)
O3	0.051 (2)	0.101 (3)	0.073 (3)	−0.0124 (19)	−0.0067 (17)	−0.012 (2)
C11	0.053 (2)	0.048 (2)	0.041 (2)	−0.0183 (18)	−0.0044 (17)	−0.0173 (18)
C12	0.073 (3)	0.054 (3)	0.072 (3)	−0.020 (2)	0.016 (3)	−0.020 (2)
C13	0.080 (4)	0.066 (3)	0.101 (5)	−0.012 (3)	0.022 (3)	−0.031 (3)
C14	0.086 (4)	0.051 (3)	0.093 (4)	−0.011 (3)	−0.001 (3)	−0.028 (3)
C15	0.101 (4)	0.050 (3)	0.098 (5)	−0.031 (3)	0.010 (4)	−0.017 (3)
C16	0.075 (3)	0.058 (3)	0.084 (4)	−0.030 (2)	0.019 (3)	−0.027 (3)
C21	0.055 (2)	0.042 (2)	0.038 (2)	−0.0174 (17)	−0.0074 (17)	−0.0140 (17)
C22	0.071 (3)	0.076 (3)	0.058 (3)	−0.039 (3)	−0.009 (2)	−0.019 (3)
C23	0.084 (4)	0.103 (4)	0.090 (5)	−0.050 (3)	−0.016 (3)	−0.039 (4)
C24	0.097 (4)	0.077 (3)	0.074 (4)	−0.033 (3)	−0.036 (3)	−0.027 (3)
C25	0.108 (4)	0.078 (3)	0.052 (3)	−0.030 (3)	−0.016 (3)	−0.029 (3)
C26	0.076 (3)	0.060 (3)	0.044 (2)	−0.024 (2)	−0.004 (2)	−0.022 (2)
C4	0.057 (2)	0.046 (2)	0.040 (2)	−0.0255 (18)	0.0003 (17)	−0.0153 (17)
O4	0.0502 (15)	0.0493 (15)	0.0433 (16)	−0.0197 (12)	−0.0026 (12)	−0.0091 (13)
C31	0.053 (2)	0.048 (2)	0.060 (3)	−0.0122 (18)	−0.002 (2)	−0.016 (2)
C32	0.056 (2)	0.048 (2)	0.055 (3)	−0.0153 (19)	−0.006 (2)	−0.011 (2)
C33	0.051 (2)	0.063 (3)	0.055 (3)	−0.024 (2)	0.009 (2)	−0.014 (2)
C34	0.057 (3)	0.077 (3)	0.070 (3)	−0.032 (2)	−0.002 (2)	−0.014 (3)
O5	0.121 (3)	0.095 (3)	0.058 (2)	−0.069 (2)	0.004 (2)	−0.020 (2)
C36	0.116 (5)	0.091 (4)	0.094 (5)	−0.054 (4)	0.007 (4)	−0.035 (4)
C37	0.172 (8)	0.108 (6)	0.106 (6)	−0.057 (6)	0.036 (6)	−0.057 (5)
C38	0.068 (3)	0.059 (3)	0.050 (3)	−0.031 (2)	0.000 (2)	−0.006 (2)
C39	0.094 (4)	0.076 (3)	0.043 (3)	−0.040 (3)	−0.002 (2)	−0.007 (2)
C40	0.098 (4)	0.103 (5)	0.059 (3)	−0.036 (4)	0.021 (3)	−0.021 (3)
C41	0.132 (6)	0.113 (5)	0.054 (3)	−0.015 (4)	0.014 (4)	−0.025 (4)

Geometric parameters (Å, º)

Re1—C1	1.929 (5)	C21—C22	1.378 (6)
Re1—C2	1.933 (5)	C21—C26	1.382 (6)
Re1—C3	1.979 (5)	C22—C23	1.396 (7)
Re1—C4	2.105 (4)	C23—C24	1.362 (9)
Re1—P1^i	2.5328 (15)	C24—C25	1.353 (8)
Re1—P1	2.5355 (14)	C25—C26	1.383 (6)
P1—C21	1.855 (4)	C4—O4	1.304 (5)
P1—C11	1.860 (4)	C4—C38	1.514 (6)
P1—Re1^i	2.5328 (15)	O4—C31	1.476 (5)
C1—O1	1.156 (5)	C31—C32	1.502 (6)
C2—O2	1.144 (5)	C32—C33	1.519 (6)
C3—O3	1.130 (5)	C33—C34	1.507 (7)
C11—C16	1.376 (6)	C34—O5	1.394 (7)
C11—C12	1.377 (6)	O5—C36	1.390 (7)
C12—C13	1.391 (7)	C36—C37	1.458 (10)
C13—C14	1.345 (8)	C38—C39	1.528 (7)
C14—C15	1.362 (8)	C39—C40	1.498 (7)
C15—C16	1.386 (7)	C40—C41	1.507 (9)
C1—Re1—C2	88.2 (2)	C11—C12—C13	120.5 (5)
C1—Re1—C3	88.57 (19)	C14—C13—C12	121.7 (6)
C2—Re1—C3	88.7 (2)	C13—C14—C15	118.8 (5)
C1—Re1—C4	90.03 (17)	C14—C15—C16	120.3 (5)
C2—Re1—C4	89.22 (19)	C11—C16—C15	121.7 (5)
C3—Re1—C4	177.52 (16)	C22—C21—C26	118.0 (4)
C1—Re1—P1^i	175.74 (14)	C22—C21—P1	121.8 (3)
C2—Re1—P1^i	95.94 (15)	C26—C21—P1	120.1 (3)
C3—Re1—P1^i	92.29 (14)	C21—C22—C23	119.9 (5)
C4—Re1—P1^i	89.27 (12)	C24—C23—C22	121.3 (6)
C1—Re1—P1	100.42 (14)	C25—C24—C23	118.9 (5)
C2—Re1—P1	171.27 (14)	C24—C25—C26	121.0 (6)
C3—Re1—P1	90.47 (14)	C21—C26—C25	120.9 (5)
C4—Re1—P1	91.79 (11)	O4—C4—C38	117.4 (4)
P1^i—Re1—P1	75.40 (4)	O4—C4—Re1	119.5 (3)
C21—P1—C11	97.52 (17)	C38—C4—Re1	123.0 (3)
C21—P1—Re1^i	113.96 (14)	C4—O4—C31	126.6 (3)
C11—P1—Re1^i	113.00 (14)	O4—C31—C32	108.9 (3)
C21—P1—Re1	114.08 (14)	C31—C32—C33	111.1 (4)
C11—P1—Re1	114.05 (14)	C34—C33—C32	110.8 (4)
Re1^i—P1—Re1	104.60 (4)	O5—C34—C33	108.2 (4)
O1—C1—Re1	175.7 (4)	C36—O5—C34	115.5 (4)
O2—C2—Re1	177.8 (5)	O5—C36—C37	110.5 (6)
O3—C3—Re1	173.4 (4)	C4—C38—C39	113.8 (4)
C16—C11—C12	117.0 (4)	C40—C39—C38	113.0 (5)
C16—C11—P1	121.3 (3)	C39—C40—C41	113.8 (6)
C12—C11—P1	121.6 (3)

Symmetry code: (i) −x+2, −y, −z+1.