trans-Bis[bis­(diphenyl­phosphino)methane-κ²P,P′]dichloro­ruthenium(II) dichloro­methane disolvate acetone hemisolvate hemihydrate

The title compound, [RuCl₂(C₂₅H₂₂P₂)₂]·2CH₂Cl₂·0.5C₃H₆O·0.5H₂O, was obtained as unreacted starting material from our attempts to prepare acetyl­ide complexes of ruthenium, based on 1,4-dieth­oxy-2,5-diethynylbenzene bridging ligands, in a route towards mol­ecular wires. The complex is centrosymmetric.

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](C-C) = 0.008 Å
• Disorder in solvent or counterion
• R factor = 0.065
• wR factor = 0.166
• Data-to-parameter ratio = 19.0

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for        C30
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for        C31
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        O32
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        O33
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        C26
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      31.00 Perc.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   6 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 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
   6 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: COLLECT (Hooft, 1998); cell refinement: SCALEPACK; data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

trans-Bis[bis(diphenylphosphino)methane-κ₂P,P']dichlororuthenium(II) dichloromethane disolvate acetone hemisolvate hemihydrate

Crystal data

[RuCl2(C25H22P2)2]·2CH2Cl2·0.5C3H6O·0.5H2O	Z = 1
Mr = 1170.61	F(000) = 597
Triclinic, P1	Dx = 1.465 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.9227 (3) Å	Cell parameters from 19167 reflections
b = 11.2603 (3) Å	θ = 2.9–27.5°
c = 11.6768 (2) Å	µ = 0.76 mm^−1
α = 92.561 (2)°	T = 173 K
β = 105.098 (1)°	Block, yellow
γ = 105.397 (1)°	0.30 × 0.30 × 0.25 mm
V = 1326.79 (6) Å^3

Data collection

Bruker–Nonius KappaCCD diffractometer	5247 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.029
Horizonally mounted graphite crystal monochromator	θmax = 27.4°, θmin = 3.1°
Detector resolution: 9 pixels mm^-1	h = −14→13
φ? ω? scans	k = −12→14
9274 measured reflections	l = −14→15
6011 independent reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.066	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.166	H-atom parameters constrained
S = 1.09	w = 1/[σ^2(Fo^2) + (0.0603P)^2 + 6.4786P] where P = (Fo^2 + 2Fc^2)/3
6011 reflections	(Δ/σ)max < 0.001
316 parameters	Δρmax = 1.35 e Å^−3
3 restraints	Δρmin = −1.10 e Å^−3

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	Occ. (<1)
Ru1	0.5000	0.5000	0.5000	0.02026 (14)
P3	0.69505 (11)	0.66032 (10)	0.50980 (10)	0.0223 (2)
Cl4	0.63983 (10)	0.37387 (10)	0.46761 (10)	0.0280 (2)
P2	0.36436 (11)	0.45710 (10)	0.30322 (10)	0.0225 (2)
C13	0.7251 (4)	0.8283 (4)	0.5398 (4)	0.0259 (9)
C7	0.3906 (4)	0.3509 (4)	0.1955 (4)	0.0264 (9)
C23	0.9760 (6)	0.6184 (5)	0.3457 (6)	0.0424 (13)
H23	1.0563	0.5961	0.3651	0.051*
C2	0.3744 (5)	0.6965 (4)	0.2415 (4)	0.0329 (10)
H2	0.4437	0.7249	0.3138	0.039*
C1	0.3129 (4)	0.5699 (4)	0.2090 (4)	0.0258 (9)
C19	0.7911 (4)	0.6541 (4)	0.4042 (4)	0.0265 (9)
C24	0.9080 (5)	0.6205 (4)	0.4310 (5)	0.0345 (11)
H24	0.9418	0.5988	0.5081	0.041*
C18	0.6257 (5)	0.8784 (4)	0.5516 (5)	0.0331 (10)
H18	0.5377	0.8263	0.5366	0.040*
C14	0.8539 (5)	0.9063 (5)	0.5625 (5)	0.0383 (12)
H14	0.9228	0.8727	0.5545	0.046*
C3	0.3350 (6)	0.7806 (5)	0.1689 (5)	0.0433 (13)
H3	0.3781	0.8668	0.1910	0.052*
C6	0.2105 (5)	0.5294 (5)	0.1022 (5)	0.0347 (10)
H6	0.1686	0.4432	0.0787	0.042*
C12	0.4838 (6)	0.4005 (5)	0.1354 (5)	0.0400 (12)
H12	0.5282	0.4869	0.1494	0.048*
C8	0.3299 (6)	0.2244 (5)	0.1757 (5)	0.0413 (12)
H8	0.2675	0.1885	0.2169	0.050*
C17	0.6547 (5)	1.0065 (5)	0.5856 (5)	0.0401 (12)
H17	0.5861	1.0408	0.5933	0.048*
C9	0.3602 (7)	0.1493 (5)	0.0949 (5)	0.0481 (14)
H9	0.3177	0.0625	0.0815	0.058*
C4	0.2331 (6)	0.7405 (5)	0.0642 (5)	0.0430 (13)
H4	0.2060	0.7991	0.0150	0.052*
C20	0.7429 (5)	0.6842 (6)	0.2906 (5)	0.0407 (12)
H20	0.6630	0.7073	0.2711	0.049*
C16	0.7818 (6)	1.0820 (5)	0.6078 (5)	0.0440 (13)
H16	0.8012	1.1684	0.6309	0.053*
C5	0.1705 (6)	0.6149 (6)	0.0309 (5)	0.0413 (12)
H5	0.1002	0.5875	−0.0409	0.050*
C10	0.4502 (6)	0.1989 (6)	0.0351 (5)	0.0465 (14)
H10	0.4697	0.1472	−0.0200	0.056*
C15	0.8819 (6)	1.0324 (5)	0.5965 (6)	0.0463 (14)
H15	0.9698	1.0849	0.6120	0.056*
C22	0.9272 (6)	0.6485 (5)	0.2334 (5)	0.0463 (14)
H22	0.9739	0.6469	0.1755	0.056*
C21	0.8105 (6)	0.6810 (6)	0.2044 (5)	0.0483 (15)
H21	0.7764	0.7011	0.1266	0.058*
C11	0.5121 (6)	0.3242 (6)	0.0553 (6)	0.0494 (15)
H11	0.5749	0.3591	0.0140	0.059*
C25	0.7859 (4)	0.6256 (4)	0.6560 (4)	0.0268 (9)
H25A	0.8422	0.5716	0.6480	0.032*
H25B	0.8390	0.7015	0.7118	0.032*
Cl27	0.8462 (4)	0.2641 (4)	0.2657 (3)	0.1404 (14)
Cl28	0.6835 (5)	0.0173 (3)	0.2486 (4)	0.1670 (18)
C26	0.7154 (12)	0.1683 (10)	0.2982 (10)	0.102 (3)
H26A	0.7314	0.1769	0.3860	0.122*
H26B	0.6359	0.1952	0.2631	0.122*
C31	0.012 (2)	1.0151 (13)	0.902 (2)	0.116 (4)	0.50
H31B	0.0126	0.9744	0.8265	0.174*	0.50
H31A	0.0972	1.0780	0.9374	0.174*	0.50
H31C	−0.0594	1.0547	0.8878	0.174*	0.50
O29	−0.0286 (14)	0.8121 (11)	0.9547 (16)	0.116 (4)	0.50
C30	−0.009 (2)	0.9209 (13)	0.9862 (14)	0.116 (4)	0.50
O32	0.033 (2)	0.953 (2)	0.8984 (19)	0.063 (5)*	0.25
O33	−0.020 (2)	1.0597 (19)	0.9104 (18)	0.055 (4)*	0.25

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ru1	0.0208 (2)	0.0192 (2)	0.0223 (2)	0.00516 (17)	0.00985 (18)	−0.00033 (17)
P3	0.0224 (5)	0.0215 (5)	0.0249 (5)	0.0053 (4)	0.0112 (4)	0.0012 (4)
Cl4	0.0268 (5)	0.0254 (5)	0.0358 (6)	0.0098 (4)	0.0141 (4)	−0.0007 (4)
P2	0.0238 (5)	0.0216 (5)	0.0228 (5)	0.0051 (4)	0.0096 (4)	0.0005 (4)
C13	0.029 (2)	0.023 (2)	0.025 (2)	0.0042 (17)	0.0096 (17)	−0.0002 (16)
C7	0.028 (2)	0.026 (2)	0.023 (2)	0.0069 (17)	0.0055 (17)	−0.0017 (16)
C23	0.047 (3)	0.031 (3)	0.065 (4)	0.016 (2)	0.039 (3)	0.006 (2)
C2	0.041 (3)	0.028 (2)	0.031 (2)	0.011 (2)	0.012 (2)	0.0011 (19)
C1	0.026 (2)	0.029 (2)	0.025 (2)	0.0093 (18)	0.0108 (17)	0.0047 (17)
C19	0.028 (2)	0.023 (2)	0.030 (2)	0.0030 (17)	0.0164 (18)	−0.0020 (17)
C24	0.037 (3)	0.027 (2)	0.051 (3)	0.011 (2)	0.029 (2)	0.012 (2)
C18	0.027 (2)	0.027 (2)	0.042 (3)	0.0062 (18)	0.008 (2)	−0.003 (2)
C14	0.031 (2)	0.037 (3)	0.049 (3)	0.004 (2)	0.020 (2)	−0.003 (2)
C3	0.066 (4)	0.026 (2)	0.047 (3)	0.020 (2)	0.024 (3)	0.006 (2)
C6	0.031 (2)	0.036 (3)	0.036 (3)	0.008 (2)	0.008 (2)	0.007 (2)
C12	0.043 (3)	0.034 (3)	0.046 (3)	0.003 (2)	0.027 (2)	−0.003 (2)
C8	0.058 (3)	0.030 (3)	0.036 (3)	0.003 (2)	0.024 (3)	−0.003 (2)
C17	0.038 (3)	0.028 (2)	0.051 (3)	0.011 (2)	0.008 (2)	−0.010 (2)
C9	0.066 (4)	0.032 (3)	0.045 (3)	0.009 (3)	0.021 (3)	−0.010 (2)
C4	0.055 (3)	0.045 (3)	0.043 (3)	0.030 (3)	0.021 (3)	0.016 (2)
C20	0.027 (2)	0.059 (3)	0.035 (3)	0.008 (2)	0.012 (2)	0.005 (2)
C16	0.047 (3)	0.024 (2)	0.056 (3)	0.003 (2)	0.016 (3)	−0.008 (2)
C5	0.037 (3)	0.051 (3)	0.040 (3)	0.019 (2)	0.011 (2)	0.014 (2)
C10	0.060 (4)	0.048 (3)	0.041 (3)	0.022 (3)	0.025 (3)	−0.007 (2)
C15	0.043 (3)	0.027 (3)	0.065 (4)	−0.005 (2)	0.024 (3)	−0.008 (2)
C22	0.050 (3)	0.039 (3)	0.050 (3)	−0.003 (2)	0.034 (3)	−0.012 (2)
C21	0.039 (3)	0.072 (4)	0.028 (3)	0.001 (3)	0.017 (2)	0.000 (3)
C11	0.051 (3)	0.053 (3)	0.052 (3)	0.012 (3)	0.034 (3)	−0.004 (3)
C25	0.021 (2)	0.027 (2)	0.032 (2)	0.0041 (17)	0.0096 (17)	0.0030 (18)
Cl27	0.122 (3)	0.153 (3)	0.107 (2)	−0.019 (2)	0.0259 (19)	0.013 (2)
Cl28	0.215 (5)	0.084 (2)	0.178 (4)	0.020 (3)	0.046 (3)	−0.032 (2)
C26	0.120 (9)	0.100 (8)	0.091 (7)	0.045 (7)	0.027 (6)	0.008 (6)
C31	0.073 (6)	0.087 (7)	0.194 (14)	0.035 (6)	0.037 (7)	0.024 (8)
O29	0.073 (6)	0.087 (7)	0.194 (14)	0.035 (6)	0.037 (7)	0.024 (8)
C30	0.073 (6)	0.087 (7)	0.194 (14)	0.035 (6)	0.037 (7)	0.024 (8)

Geometric parameters (Å, º)

Ru1—P2^i	2.3357 (11)	C12—H12	0.9500
Ru1—P2	2.3357 (11)	C8—C9	1.398 (7)
Ru1—P3	2.3713 (11)	C8—H8	0.9500
Ru1—P3^i	2.3713 (11)	C17—C16	1.373 (8)
Ru1—Cl4	2.4285 (10)	C17—H17	0.9500
Ru1—Cl4^i	2.4285 (10)	C9—C10	1.367 (8)
P3—C19	1.825 (4)	C9—H9	0.9500
P3—C13	1.833 (4)	C4—C5	1.384 (8)
P3—C25	1.853 (5)	C4—H4	0.9500
P2—C1	1.822 (5)	C20—C21	1.399 (7)
P2—C7	1.824 (4)	C20—H20	0.9500
P2—C25^i	1.850 (4)	C16—C15	1.384 (8)
C13—C18	1.383 (6)	C16—H16	0.9500
C13—C14	1.396 (7)	C5—H5	0.9500
C7—C8	1.383 (7)	C10—C11	1.372 (9)
C7—C12	1.395 (7)	C10—H10	0.9500
C23—C22	1.374 (9)	C15—H15	0.9500
C23—C24	1.391 (7)	C22—C21	1.381 (9)
C23—H23	0.9500	C22—H22	0.9500
C2—C3	1.378 (7)	C21—H21	0.9500
C2—C1	1.392 (6)	C11—H11	0.9500
C2—H2	0.9500	C25—P2^i	1.850 (4)
C1—C6	1.402 (7)	C25—H25A	0.9900
C19—C20	1.387 (7)	C25—H25B	0.9900
C19—C24	1.389 (7)	Cl27—C26	1.689 (12)
C24—H24	0.9500	Cl28—C26	1.685 (11)
C18—C17	1.406 (7)	C26—H26A	0.9900
C18—H18	0.9500	C26—H26B	0.9900
C14—C15	1.388 (7)	C31—C30	1.4900 (10)
C14—H14	0.9500	C31—H31B	0.9800
C3—C4	1.384 (9)	C31—H31A	0.9800
C3—H3	0.9500	C31—H31C	0.9800
C6—C5	1.385 (7)	O29—C30	1.2098 (10)
C6—H6	0.9500	C30—C31^ii	1.47 (3)
C12—C11	1.388 (7)	O32—O33	1.49 (3)
P2^i—Ru1—P2	180.0	C11—C12—C7	120.4 (5)
P2^i—Ru1—P3	71.03 (4)	C11—C12—H12	119.8
P2—Ru1—P3	108.97 (4)	C7—C12—H12	119.8
P2^i—Ru1—P3^i	108.97 (4)	C7—C8—C9	120.1 (5)
P2—Ru1—P3^i	71.03 (4)	C7—C8—H8	120.0
P3—Ru1—P3^i	180.0	C9—C8—H8	120.0
P2^i—Ru1—Cl4	85.39 (4)	C16—C17—C18	120.1 (5)
P2—Ru1—Cl4	94.61 (4)	C16—C17—H17	120.0
P3—Ru1—Cl4	80.81 (4)	C18—C17—H17	120.0
P3^i—Ru1—Cl4	99.19 (4)	C10—C9—C8	120.9 (5)
P2^i—Ru1—Cl4^i	94.61 (4)	C10—C9—H9	119.5
P2—Ru1—Cl4^i	85.39 (4)	C8—C9—H9	119.5
P3—Ru1—Cl4^i	99.19 (4)	C3—C4—C5	120.1 (5)
P3^i—Ru1—Cl4^i	80.81 (4)	C3—C4—H4	120.0
Cl4—Ru1—Cl4^i	180.00 (5)	C5—C4—H4	120.0
C19—P3—C13	100.8 (2)	C19—C20—C21	120.8 (5)
C19—P3—C25	108.5 (2)	C19—C20—H20	119.6
C13—P3—C25	101.1 (2)	C21—C20—H20	119.6
C19—P3—Ru1	121.43 (15)	C17—C16—C15	120.1 (5)
C13—P3—Ru1	128.14 (15)	C17—C16—H16	119.9
C25—P3—Ru1	93.08 (14)	C15—C16—H16	119.9
C1—P2—C7	101.5 (2)	C4—C5—C6	119.9 (5)
C1—P2—C25^i	104.5 (2)	C4—C5—H5	120.0
C7—P2—C25^i	107.3 (2)	C6—C5—H5	120.0
C1—P2—Ru1	126.29 (15)	C9—C10—C11	119.4 (5)
C7—P2—Ru1	120.24 (15)	C9—C10—H10	120.3
C25^i—P2—Ru1	94.34 (15)	C11—C10—H10	120.3
C18—C13—C14	119.2 (4)	C16—C15—C14	120.1 (5)
C18—C13—P3	121.4 (3)	C16—C15—H15	120.0
C14—C13—P3	119.1 (4)	C14—C15—H15	120.0
C8—C7—C12	118.6 (4)	C23—C22—C21	120.4 (5)
C8—C7—P2	124.0 (4)	C23—C22—H22	119.8
C12—C7—P2	117.3 (4)	C21—C22—H22	119.8
C22—C23—C24	120.1 (5)	C22—C21—C20	119.4 (6)
C22—C23—H23	119.9	C22—C21—H21	120.3
C24—C23—H23	119.9	C20—C21—H21	120.3
C3—C2—C1	120.1 (5)	C10—C11—C12	120.7 (5)
C3—C2—H2	119.9	C10—C11—H11	119.7
C1—C2—H2	119.9	C12—C11—H11	119.7
C2—C1—C6	119.2 (4)	P2^i—C25—P3	95.2 (2)
C2—C1—P2	120.8 (4)	P2^i—C25—H25A	112.7
C6—C1—P2	119.9 (4)	P3—C25—H25A	112.7
C20—C19—C24	118.7 (4)	P2^i—C25—H25B	112.7
C20—C19—P3	117.4 (4)	P3—C25—H25B	112.7
C24—C19—P3	123.9 (4)	H25A—C25—H25B	110.2
C19—C24—C23	120.6 (5)	Cl28—C26—Cl27	114.7 (7)
C19—C24—H24	119.7	Cl28—C26—H26A	108.6
C23—C24—H24	119.7	Cl27—C26—H26A	108.6
C13—C18—C17	120.1 (5)	Cl28—C26—H26B	108.6
C13—C18—H18	119.9	Cl27—C26—H26B	108.6
C17—C18—H18	119.9	H26A—C26—H26B	107.6
C15—C14—C13	120.4 (5)	C30—C31—H31B	109.5
C15—C14—H14	119.8	C30—C31—H31A	109.5
C13—C14—H14	119.8	H31B—C31—H31A	109.5
C2—C3—C4	120.5 (5)	C30—C31—H31C	109.5
C2—C3—H3	119.7	H31B—C31—H31C	109.5
C4—C3—H3	119.7	H31A—C31—H31C	109.5
C5—C6—C1	120.1 (5)	O29—C30—C31^ii	131.3 (16)
C5—C6—H6	120.0	O29—C30—C31	120.66 (14)
C1—C6—H6	120.0	C31^ii—C30—C31	107.9 (16)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+2, −z+2.