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The mixed-valence complex, [Ru2(C2H4NO)4(H2O)2]ClO4, contains two centrosymmetric cations with Ru—Ru bond distances of 2.2817 (10) and 2.2804 (10) Å. The diruthenium cations and perchlorate anions are inter­connected by N—H...O and O—H...O hydrogen bonds into a two-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806039298/kp2034sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806039298/kp2034Isup2.hkl
Contains datablock I

CCDC reference: 627962

Key indicators

  • Single-crystal X-ray study
  • T = 123 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.031
  • wR factor = 0.069
  • Data-to-parameter ratio = 16.7

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl1 PLAT354_ALERT_3_C Short O-H Bond (0.82A) O5 - H3 ... 0.69 Ang. PLAT354_ALERT_3_C Short O-H Bond (0.82A) O6 - H8 ... 0.71 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 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 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: CrystalClear (Molecular Structure Corporation & Rigaku, 2001); cell refinement: CrystalClear; data reduction: TEXSAN (Rigaku/MSC, 2004); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97 and TEXSAN.

Tetra-µ-acetamidato-κ4N:O;κ4O:N-diaquadiruthenium(II,III)(Ru—Ru) perchlorate top
Crystal data top
[Ru2(C2H4NO)4(H2O)2]ClO4Z = 2
Mr = 569.87F(000) = 562
Triclinic, P1Dx = 2.091 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71069 Å
a = 7.704 (4) ÅCell parameters from 2208 reflections
b = 11.454 (6) Åθ = 3.5–27.5°
c = 11.686 (6) ŵ = 1.87 mm1
α = 109.882 (4)°T = 123 K
β = 98.696 (4)°Block, brown
γ = 104.705 (4)°0.18 × 0.12 × 0.12 mm
V = 905.4 (8) Å3
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
4086 independent reflections
Graphite monochromator3025 reflections with I > 2σ(I)
Detector resolution: 14.62 pixels mm-1Rint = 0.022
ω scansθmax = 27.5°, θmin = 3.5°
Absorption correction: integration
(ABSCOR; Higashi, 1999)
h = 99
Tmin = 0.753, Tmax = 0.825k = 149
7392 measured reflectionsl = 1515
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.031H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.069 w = 1/[σ2(Fo2) + (0.0297P)2 + 0.3098P]
where P = (Fo2 + 2Fc2)/3
S = 1.11(Δ/σ)max = 0.002
4086 reflectionsΔρmax = 0.46 e Å3
244 parametersΔρmin = 0.47 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0045 (7)
Special details top

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 (Å2) top
xyzUiso*/Ueq
Ru10.38565 (3)0.51790 (2)1.04840 (2)0.00755 (9)
N10.3533 (4)0.3414 (2)1.0606 (2)0.0120 (6)
H10.26540.31171.09370.014*
O10.5789 (3)0.3046 (2)0.96454 (19)0.0124 (5)
N20.4183 (4)0.3950 (2)0.7862 (2)0.0120 (6)
H20.45070.35790.71720.014*
O20.1898 (3)0.4340 (2)0.87734 (19)0.0114 (5)
O50.1581 (4)0.5388 (3)1.1549 (2)0.0168 (6)
H30.110 (6)0.483 (4)1.161 (4)0.025*
H40.082 (6)0.566 (4)1.141 (4)0.025*
Ru20.38694 (3)0.02088 (2)0.54850 (2)0.00746 (9)
N30.6680 (4)0.1626 (2)0.4523 (2)0.0118 (6)
H50.75810.19060.42010.014*
O30.4440 (3)0.2045 (2)0.54699 (19)0.0119 (5)
N40.5813 (3)0.0960 (2)0.7154 (2)0.0100 (5)
H60.55000.13240.78510.012*
O40.8045 (3)0.0479 (2)0.62249 (19)0.0103 (5)
O60.1655 (3)0.0477 (3)0.6584 (2)0.0162 (6)
H70.070 (6)0.049 (4)0.642 (4)0.024*
H80.156 (6)0.005 (4)0.691 (4)0.024*
C10.4569 (4)0.2699 (3)1.0217 (3)0.0113 (7)
C20.4423 (5)0.1452 (3)1.0418 (3)0.0204 (8)
H90.40600.07100.96000.031*
H100.34860.13051.08810.031*
H110.56300.15271.09050.031*
C30.2464 (4)0.3909 (3)0.7764 (3)0.0095 (6)
C40.1090 (4)0.3409 (3)0.6522 (3)0.0170 (7)
H120.15990.29520.58510.026*
H130.08290.41490.63770.026*
H140.00630.27990.65190.026*
C50.5766 (4)0.2409 (3)0.4982 (3)0.0106 (6)
C60.6145 (5)0.3739 (3)0.4940 (3)0.0202 (8)
H150.50370.37680.44290.030*
H160.71870.39120.45650.030*
H170.64600.44070.57980.030*
C70.7499 (4)0.0929 (3)0.7240 (3)0.0115 (7)
C80.8862 (4)0.1385 (3)0.8479 (3)0.0157 (7)
H180.83710.18540.91550.023*
H191.00390.19760.84900.023*
H200.90720.06250.86080.023*
Cl11.00650 (12)0.24343 (9)0.25251 (8)0.01977 (18)
O70.9754 (5)0.3000 (3)0.1628 (3)0.0521 (9)
O81.1889 (4)0.2348 (4)0.2667 (4)0.0691 (12)
O90.8699 (4)0.1145 (3)0.2057 (2)0.0347 (7)
O100.9878 (4)0.3230 (3)0.3702 (2)0.0448 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.00647 (15)0.00821 (14)0.00821 (14)0.00346 (10)0.00277 (10)0.00240 (10)
N10.0119 (14)0.0106 (13)0.0149 (14)0.0027 (11)0.0070 (12)0.0060 (11)
O10.0143 (12)0.0104 (11)0.0143 (11)0.0064 (10)0.0049 (10)0.0048 (9)
N20.0131 (15)0.0113 (13)0.0116 (13)0.0055 (12)0.0047 (12)0.0025 (11)
O20.0089 (11)0.0146 (11)0.0096 (11)0.0043 (9)0.0018 (9)0.0033 (9)
O50.0143 (14)0.0227 (14)0.0231 (13)0.0105 (12)0.0117 (12)0.0143 (12)
Ru20.00630 (14)0.00844 (14)0.00785 (14)0.00333 (10)0.00296 (10)0.00235 (10)
N30.0111 (14)0.0140 (13)0.0118 (13)0.0035 (12)0.0042 (11)0.0067 (11)
O30.0126 (12)0.0116 (11)0.0139 (11)0.0052 (10)0.0056 (10)0.0059 (9)
N40.0092 (14)0.0127 (13)0.0093 (13)0.0048 (11)0.0050 (11)0.0041 (11)
O40.0091 (11)0.0122 (11)0.0092 (10)0.0045 (9)0.0032 (9)0.0027 (9)
O60.0114 (13)0.0257 (14)0.0204 (14)0.0105 (12)0.0099 (12)0.0143 (11)
C10.0084 (16)0.0098 (15)0.0112 (15)0.0010 (13)0.0011 (13)0.0018 (12)
C20.024 (2)0.0166 (17)0.029 (2)0.0111 (16)0.0121 (17)0.0141 (15)
C30.0135 (17)0.0088 (14)0.0083 (15)0.0061 (13)0.0022 (13)0.0042 (12)
C40.0143 (18)0.0212 (18)0.0143 (17)0.0084 (15)0.0015 (14)0.0047 (14)
C50.0126 (16)0.0078 (14)0.0093 (15)0.0022 (13)0.0003 (13)0.0030 (12)
C60.023 (2)0.0158 (17)0.0263 (19)0.0070 (15)0.0088 (16)0.0125 (15)
C70.0133 (17)0.0073 (14)0.0114 (16)0.0002 (13)0.0023 (14)0.0033 (12)
C80.0142 (18)0.0203 (17)0.0104 (16)0.0046 (14)0.0003 (14)0.0055 (13)
Cl10.0172 (4)0.0245 (4)0.0168 (4)0.0015 (3)0.0062 (3)0.0102 (3)
O70.076 (3)0.0372 (18)0.0255 (15)0.0136 (17)0.0044 (16)0.0219 (14)
O80.0188 (17)0.082 (3)0.094 (3)0.0177 (18)0.0122 (19)0.019 (2)
O90.0351 (17)0.0274 (15)0.0352 (16)0.0032 (13)0.0012 (13)0.0190 (13)
O100.048 (2)0.052 (2)0.0196 (14)0.0049 (16)0.0154 (14)0.0026 (14)
Geometric parameters (Å, º) top
Ru1—Ru1i2.2817 (10)N4—H60.8800
Ru1—O1i2.042 (2)O4—C71.302 (3)
Ru1—O22.060 (2)O6—H70.73 (4)
Ru1—O52.312 (2)O6—H80.71 (4)
Ru1—N12.030 (3)C1—C21.504 (4)
Ru1—N2i2.013 (3)C2—H90.9800
N1—C11.304 (4)C2—H100.9800
N1—H10.8800C2—H110.9800
O1—C11.292 (4)C3—C41.490 (4)
N2—C31.299 (4)C4—H120.9800
N2—H20.8800C4—H130.9800
O2—C31.302 (3)C4—H140.9800
O5—H30.69 (4)C5—C61.496 (4)
O5—H40.75 (4)C6—H150.9800
Ru2—Ru2ii2.2804 (10)C6—H160.9800
Ru2—O32.044 (2)C6—H170.9800
Ru2—O4ii2.058 (2)C7—C81.490 (4)
Ru2—O62.305 (2)C8—H180.9800
Ru2—N3ii2.032 (3)C8—H190.9800
Ru2—N42.027 (3)C8—H200.9800
N3—C51.302 (4)Cl1—O101.421 (3)
N3—H50.8800Cl1—O81.422 (3)
O3—C51.290 (4)Cl1—O71.429 (3)
N4—C71.299 (4)Cl1—O91.441 (3)
N2i—Ru1—N189.42 (11)Ru2—N4—H6118.6
N2i—Ru1—O1i90.42 (10)C7—O4—Ru2ii117.64 (19)
N1—Ru1—O1i179.29 (9)Ru2—O6—H7135 (3)
N2i—Ru1—O2177.97 (9)Ru2—O6—H8109 (3)
N1—Ru1—O292.36 (10)H7—O6—H8102 (4)
O1i—Ru1—O287.79 (9)O1—C1—N1120.8 (3)
N2i—Ru1—Ru1i87.85 (8)O1—C1—C2116.9 (3)
N1—Ru1—Ru1i86.68 (7)N1—C1—C2122.3 (3)
O1i—Ru1—Ru1i92.63 (6)C1—C2—H9109.5
O2—Ru1—Ru1i91.28 (7)C1—C2—H10109.5
N2i—Ru1—O590.02 (10)H9—C2—H10109.5
N1—Ru1—O587.88 (9)C1—C2—H11109.5
O1i—Ru1—O592.81 (8)H9—C2—H11109.5
O2—Ru1—O591.02 (10)H10—C2—H11109.5
Ru1i—Ru1—O5174.18 (6)N2—C3—O2120.1 (3)
C1—N1—Ru1123.0 (2)N2—C3—C4122.4 (3)
C1—N1—H1118.5O2—C3—C4117.5 (3)
Ru1—N1—H1118.5C3—C4—H12109.5
C1—O1—Ru1i116.70 (17)C3—C4—H13109.5
C3—N2—Ru1i123.2 (2)H12—C4—H13109.5
C3—N2—H2118.4C3—C4—H14109.5
Ru1i—N2—H2118.4H12—C4—H14109.5
C3—O2—Ru1117.37 (19)H13—C4—H14109.5
Ru1—O5—H3116 (3)O3—C5—N3120.6 (3)
Ru1—O5—H4126 (3)O3—C5—C6116.8 (3)
H3—O5—H4101 (4)N3—C5—C6122.6 (3)
N4—Ru2—N3ii90.65 (10)C5—C6—H15109.5
N4—Ru2—O389.68 (9)C5—C6—H16109.5
N3ii—Ru2—O3179.10 (8)H15—C6—H16109.5
N4—Ru2—O4ii177.35 (9)C5—C6—H17109.5
N3ii—Ru2—O4ii91.82 (9)H15—C6—H17109.5
O3—Ru2—O4ii87.84 (8)H16—C6—H17109.5
N4—Ru2—Ru2ii87.79 (8)N4—C7—O4120.1 (3)
N3ii—Ru2—Ru2ii86.60 (7)N4—C7—C8122.1 (3)
O3—Ru2—Ru2ii92.57 (6)O4—C7—C8117.8 (3)
O4ii—Ru2—Ru2ii91.37 (7)C7—C8—H18109.5
N4—Ru2—O688.73 (10)C7—C8—H19109.5
N3ii—Ru2—O687.73 (9)H18—C8—H19109.5
O3—Ru2—O693.12 (8)C7—C8—H20109.5
O4ii—Ru2—O692.35 (10)H18—C8—H20109.5
Ru2ii—Ru2—O6173.31 (6)H19—C8—H20109.5
C5—N3—Ru2ii123.3 (2)O10—Cl1—O8109.9 (2)
C5—N3—H5118.4O10—Cl1—O7109.8 (2)
Ru2ii—N3—H5118.4O8—Cl1—O7108.8 (2)
C5—O3—Ru2116.93 (17)O10—Cl1—O9109.70 (18)
C7—N4—Ru2122.9 (2)O8—Cl1—O9110.4 (2)
C7—N4—H6118.6O7—Cl1—O9108.15 (17)
N2i—Ru1—N1—C185.6 (3)Ru1i—O1—C1—N14.8 (4)
O2—Ru1—N1—C193.4 (3)Ru1i—O1—C1—C2174.7 (2)
Ru1i—Ru1—N1—C12.3 (2)Ru1—N1—C1—O14.9 (4)
O5—Ru1—N1—C1175.6 (3)Ru1—N1—C1—C2174.5 (2)
N1—Ru1—O2—C387.0 (2)Ru1i—N2—C3—O26.2 (4)
O1i—Ru1—O2—C392.3 (2)Ru1i—N2—C3—C4172.2 (2)
Ru1i—Ru1—O2—C30.2 (2)Ru1—O2—C3—N23.8 (4)
O5—Ru1—O2—C3174.9 (2)Ru1—O2—C3—C4174.7 (2)
N4—Ru2—O3—C587.4 (2)Ru2—O3—C5—N30.1 (4)
O4ii—Ru2—O3—C591.7 (2)Ru2—O3—C5—C6178.3 (2)
Ru2ii—Ru2—O3—C50.4 (2)Ru2ii—N3—C5—O30.3 (4)
O6—Ru2—O3—C5176.1 (2)Ru2ii—N3—C5—C6177.8 (2)
N3ii—Ru2—N4—C781.9 (3)Ru2—N4—C7—O44.7 (4)
O3—Ru2—N4—C797.2 (3)Ru2—N4—C7—C8174.8 (2)
Ru2ii—Ru2—N4—C74.6 (2)Ru2ii—O4—C7—N41.5 (4)
O6—Ru2—N4—C7169.7 (3)Ru2ii—O4—C7—C8178.0 (2)
Symmetry codes: (i) x+1, y+1, z+2; (ii) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H4···O2iii0.75 (4)2.07 (4)2.761 (3)152 (4)
O5—H3···O7iv0.69 (4)2.09 (4)2.780 (4)173 (4)
O6—H7···O4v0.73 (4)2.02 (4)2.750 (3)171 (4)
O6—H8···O9ii0.71 (4)2.10 (4)2.816 (4)178 (4)
N1—H1···O7iv0.882.483.296 (4)155
N1—H1···O8iv0.882.553.321 (5)146
N2—H2···O30.882.142.975 (3)158
N3—H5···O100.882.313.159 (4)163
N4—H6···O10.882.273.081 (3)153
Symmetry codes: (ii) x+1, y, z+1; (iii) x, y+1, z+2; (iv) x1, y, z+1; (v) x1, y, z.
 

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