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The asymmetric unit of the title mixed-valence complex, [Ru
2(C
2H
4NO)
4(H
2O)
2](C
24H
20B)·H
2O, comprises half each of two centrosymmetric cations, with Ru—Ru bond distances of 2.2823 (5) and 2.2742 (5) Å, a tetraphenylborate anion and a water molecule. N—H
O and O—H
O hydrogen bonds connect the diruthenium units into a chain.
Supporting information
CCDC reference: 627964
Key indicators
- Single-crystal X-ray study
- T = 123 K
- Mean (C-C) = 0.003 Å
- R factor = 0.027
- wR factor = 0.059
- Data-to-parameter ratio = 17.3
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor O6 - H8 ... ?
PLAT420_ALERT_2_B D-H Without Acceptor O7 - H41 ... ?
PLAT420_ALERT_2_B D-H Without Acceptor O7 - H42 ... ?
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru2 - O6 .. 5.94 su
PLAT354_ALERT_3_C Short O-H Bond (0.82A) O7 - H42 ... 0.70 Ang.
PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2 ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N4 - H4 ... ?
0 ALERT level A = In general: serious problem
3 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
6 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 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
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-bis[aquaruthenium(II,III)](Ru—Ru) tetraphenylborate monohydrate
top
Crystal data top
[Ru2(C2H4NO)4(H2O)2]C24H20B·H2O | Z = 2 |
Mr = 807.65 | F(000) = 822 |
Triclinic, P1 | Dx = 1.585 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 9.562 (2) Å | Cell parameters from 5667 reflections |
b = 13.554 (3) Å | θ = 3.0–27.5° |
c = 13.848 (3) Å | µ = 0.94 mm−1 |
α = 77.739 (6)° | T = 123 K |
β = 84.236 (8)° | Block, brown |
γ = 75.068 (7)° | 0.45 × 0.35 × 0.35 mm |
V = 1692.6 (6) Å3 | |
Data collection top
Rigaku/MSC Mercury CCD area-detector diffractometer | 7680 independent reflections |
Graphite monochromator | 6970 reflections with I > 2σ(I) |
Detector resolution: 14.62 pixels mm-1 | Rint = 0.024 |
ω scans | θmax = 27.5°, θmin = 3.0° |
Absorption correction: integration (NUMABS; Higashi, 1999) | h = −11→12 |
Tmin = 0.676, Tmax = 0.734 | k = −17→12 |
13834 measured reflections | l = −16→17 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.059 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0182P)2 + 1.827P] where P = (Fo2 + 2Fc2)/3 |
7680 reflections | (Δ/σ)max = 0.002 |
443 parameters | Δρmax = 0.62 e Å−3 |
0 restraints | Δρmin = −0.52 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Ru1 | 0.547048 (17) | 0.454408 (13) | 0.073517 (12) | 0.01090 (5) | |
Ru2 | 0.428019 (17) | 0.507846 (13) | 0.436870 (12) | 0.00979 (5) | |
N1 | 0.55817 (19) | 0.32355 (14) | 0.02148 (13) | 0.0147 (4) | |
H1 | 0.5906 | 0.2629 | 0.0602 | 0.018* | |
O1 | 0.46844 (16) | 0.41227 (12) | −0.12486 (11) | 0.0157 (3) | |
N2 | 0.25397 (18) | 0.53846 (14) | −0.01114 (13) | 0.0145 (4) | |
H2 | 0.1779 | 0.5668 | −0.0472 | 0.017* | |
O2 | 0.34425 (15) | 0.45274 (12) | 0.13580 (11) | 0.0153 (3) | |
N3 | 0.58033 (19) | 0.55981 (14) | 0.34216 (13) | 0.0134 (4) | |
H3 | 0.5677 | 0.5740 | 0.2781 | 0.016* | |
O3 | 0.72264 (15) | 0.54834 (12) | 0.46671 (11) | 0.0140 (3) | |
N4 | 0.66468 (19) | 0.34460 (14) | 0.54395 (13) | 0.0141 (4) | |
H4 | 0.7350 | 0.3066 | 0.5821 | 0.017* | |
O4 | 0.52500 (15) | 0.35925 (11) | 0.41747 (11) | 0.0127 (3) | |
O5 | 0.64117 (18) | 0.35875 (14) | 0.21999 (12) | 0.0176 (3) | |
H5 | 0.603 (3) | 0.363 (2) | 0.274 (3) | 0.034 (9)* | |
H6 | 0.666 (3) | 0.296 (3) | 0.221 (2) | 0.038 (9)* | |
O6 | 0.26932 (18) | 0.51407 (14) | 0.31764 (13) | 0.0182 (3) | |
H7 | 0.302 (3) | 0.496 (2) | 0.264 (3) | 0.036 (9)* | |
H8 | 0.221 (3) | 0.470 (3) | 0.344 (2) | 0.039 (9)* | |
C1 | 0.5199 (2) | 0.32461 (17) | −0.06606 (16) | 0.0147 (4) | |
C2 | 0.5302 (3) | 0.22760 (18) | −0.10425 (18) | 0.0219 (5) | |
H9 | 0.5734 | 0.2348 | −0.1718 | 0.033* | |
H10 | 0.4330 | 0.2163 | −0.1043 | 0.033* | |
H11 | 0.5909 | 0.1681 | −0.0616 | 0.033* | |
C3 | 0.2346 (2) | 0.49359 (16) | 0.08032 (16) | 0.0136 (4) | |
C4 | 0.0896 (2) | 0.48476 (18) | 0.12778 (17) | 0.0192 (5) | |
H12 | 0.0146 | 0.5185 | 0.0799 | 0.029* | |
H13 | 0.0700 | 0.5189 | 0.1851 | 0.029* | |
H14 | 0.0893 | 0.4111 | 0.1494 | 0.029* | |
C5 | 0.6971 (2) | 0.57267 (16) | 0.37420 (15) | 0.0129 (4) | |
C6 | 0.8056 (2) | 0.61811 (19) | 0.30548 (17) | 0.0203 (5) | |
H15 | 0.9035 | 0.5829 | 0.3273 | 0.030* | |
H16 | 0.7871 | 0.6926 | 0.3059 | 0.030* | |
H17 | 0.7971 | 0.6085 | 0.2383 | 0.030* | |
C7 | 0.6245 (2) | 0.30406 (16) | 0.47774 (15) | 0.0129 (4) | |
C8 | 0.6882 (2) | 0.19384 (17) | 0.46593 (17) | 0.0181 (5) | |
H18 | 0.6099 | 0.1596 | 0.4647 | 0.027* | |
H19 | 0.7491 | 0.1566 | 0.5215 | 0.027* | |
H20 | 0.7471 | 0.1932 | 0.4038 | 0.027* | |
B1 | 0.2034 (3) | 0.08923 (19) | 0.23457 (18) | 0.0141 (5) | |
C9 | 0.1470 (2) | 0.14078 (16) | 0.12274 (16) | 0.0144 (4) | |
C10 | 0.0512 (2) | 0.10692 (18) | 0.07426 (17) | 0.0183 (5) | |
H21 | 0.0165 | 0.0482 | 0.1073 | 0.022* | |
C11 | 0.0047 (3) | 0.15576 (19) | −0.02036 (18) | 0.0214 (5) | |
H22 | −0.0610 | 0.1307 | −0.0502 | 0.026* | |
C12 | 0.0544 (3) | 0.24067 (19) | −0.07046 (18) | 0.0225 (5) | |
H23 | 0.0233 | 0.2745 | −0.1348 | 0.027* | |
C13 | 0.1506 (2) | 0.27601 (18) | −0.02550 (18) | 0.0206 (5) | |
H24 | 0.1862 | 0.3339 | −0.0595 | 0.025* | |
C14 | 0.1948 (2) | 0.22712 (17) | 0.06871 (17) | 0.0168 (4) | |
H25 | 0.2601 | 0.2530 | 0.0980 | 0.020* | |
C15 | 0.1243 (2) | −0.00530 (16) | 0.28536 (16) | 0.0141 (4) | |
C16 | 0.1623 (2) | −0.09801 (18) | 0.24843 (17) | 0.0181 (5) | |
H26 | 0.2320 | −0.1032 | 0.1947 | 0.022* | |
C17 | 0.1031 (3) | −0.18215 (18) | 0.28657 (18) | 0.0214 (5) | |
H27 | 0.1318 | −0.2431 | 0.2588 | 0.026* | |
C18 | 0.0016 (3) | −0.17720 (19) | 0.36558 (18) | 0.0230 (5) | |
H28 | −0.0390 | −0.2347 | 0.3927 | 0.028* | |
C19 | −0.0395 (3) | −0.0875 (2) | 0.40436 (18) | 0.0225 (5) | |
H29 | −0.1093 | −0.0831 | 0.4582 | 0.027* | |
C20 | 0.0209 (2) | −0.00309 (18) | 0.36475 (17) | 0.0171 (4) | |
H30 | −0.0091 | 0.0578 | 0.3925 | 0.021* | |
C21 | 0.1611 (2) | 0.18331 (17) | 0.29803 (16) | 0.0147 (4) | |
C22 | 0.0189 (2) | 0.24657 (17) | 0.29723 (17) | 0.0174 (4) | |
H31 | −0.0485 | 0.2349 | 0.2576 | 0.021* | |
C23 | −0.0278 (2) | 0.32530 (17) | 0.35158 (18) | 0.0195 (5) | |
H32 | −0.1251 | 0.3658 | 0.3486 | 0.023* | |
C24 | 0.0678 (3) | 0.34476 (18) | 0.41026 (18) | 0.0217 (5) | |
H33 | 0.0367 | 0.3978 | 0.4483 | 0.026* | |
C25 | 0.2098 (3) | 0.28512 (19) | 0.41228 (18) | 0.0237 (5) | |
H34 | 0.2767 | 0.2974 | 0.4520 | 0.028* | |
C26 | 0.2547 (2) | 0.20699 (19) | 0.35604 (17) | 0.0199 (5) | |
H35 | 0.3530 | 0.1685 | 0.3574 | 0.024* | |
C27 | 0.3790 (2) | 0.03495 (17) | 0.22952 (17) | 0.0151 (4) | |
C28 | 0.4644 (2) | 0.02999 (17) | 0.14138 (17) | 0.0163 (4) | |
H36 | 0.4212 | 0.0639 | 0.0804 | 0.020* | |
C29 | 0.6113 (2) | −0.02314 (18) | 0.13986 (18) | 0.0196 (5) | |
H37 | 0.6653 | −0.0255 | 0.0786 | 0.024* | |
C30 | 0.6776 (2) | −0.07215 (19) | 0.22785 (19) | 0.0231 (5) | |
H38 | 0.7772 | −0.1078 | 0.2273 | 0.028* | |
C31 | 0.5969 (3) | −0.0686 (2) | 0.31667 (19) | 0.0252 (5) | |
H39 | 0.6413 | −0.1014 | 0.3775 | 0.030* | |
C32 | 0.4506 (2) | −0.01678 (18) | 0.31639 (18) | 0.0209 (5) | |
H40 | 0.3968 | −0.0165 | 0.3779 | 0.025* | |
O7 | 0.7267 (3) | 0.16188 (17) | 0.1909 (2) | 0.0380 (5) | |
H41 | 0.692 (4) | 0.118 (3) | 0.210 (3) | 0.057 (14)* | |
H42 | 0.801 (6) | 0.140 (4) | 0.184 (4) | 0.09 (2)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ru1 | 0.01145 (8) | 0.01374 (9) | 0.00713 (8) | −0.00183 (6) | −0.00078 (6) | −0.00255 (6) |
Ru2 | 0.01091 (8) | 0.01144 (8) | 0.00635 (8) | −0.00144 (6) | −0.00127 (6) | −0.00143 (6) |
N1 | 0.0169 (9) | 0.0137 (9) | 0.0129 (9) | −0.0026 (7) | 0.0004 (7) | −0.0031 (7) |
O1 | 0.0196 (7) | 0.0160 (8) | 0.0118 (7) | −0.0024 (6) | −0.0025 (6) | −0.0049 (6) |
N2 | 0.0114 (8) | 0.0179 (9) | 0.0135 (9) | −0.0022 (7) | −0.0032 (7) | −0.0022 (7) |
O2 | 0.0133 (7) | 0.0207 (8) | 0.0105 (7) | −0.0028 (6) | 0.0003 (6) | −0.0022 (6) |
N3 | 0.0170 (9) | 0.0157 (9) | 0.0068 (8) | −0.0040 (7) | 0.0002 (7) | −0.0011 (7) |
O3 | 0.0137 (7) | 0.0172 (8) | 0.0114 (7) | −0.0043 (6) | 0.0002 (6) | −0.0029 (6) |
N4 | 0.0142 (8) | 0.0136 (9) | 0.0120 (9) | 0.0006 (7) | −0.0030 (7) | −0.0012 (7) |
O4 | 0.0149 (7) | 0.0118 (7) | 0.0104 (7) | −0.0010 (6) | −0.0026 (5) | −0.0021 (6) |
O5 | 0.0216 (8) | 0.0178 (9) | 0.0102 (8) | 0.0004 (7) | −0.0016 (6) | −0.0020 (6) |
O6 | 0.0189 (8) | 0.0249 (9) | 0.0119 (8) | −0.0052 (7) | −0.0019 (6) | −0.0054 (7) |
C1 | 0.0133 (10) | 0.0169 (11) | 0.0141 (11) | −0.0037 (8) | 0.0009 (8) | −0.0044 (8) |
C2 | 0.0262 (12) | 0.0199 (12) | 0.0210 (12) | −0.0037 (10) | −0.0015 (9) | −0.0094 (10) |
C3 | 0.0141 (10) | 0.0142 (10) | 0.0132 (10) | −0.0035 (8) | 0.0006 (8) | −0.0045 (8) |
C4 | 0.0142 (10) | 0.0226 (12) | 0.0186 (12) | −0.0037 (9) | 0.0026 (8) | −0.0020 (9) |
C5 | 0.0157 (10) | 0.0099 (10) | 0.0116 (10) | −0.0012 (8) | 0.0023 (8) | −0.0027 (8) |
C6 | 0.0219 (11) | 0.0236 (12) | 0.0161 (11) | −0.0104 (9) | 0.0045 (9) | −0.0018 (9) |
C7 | 0.0132 (9) | 0.0133 (10) | 0.0105 (10) | −0.0039 (8) | 0.0029 (7) | 0.0007 (8) |
C8 | 0.0221 (11) | 0.0115 (10) | 0.0193 (12) | −0.0011 (9) | −0.0023 (9) | −0.0030 (9) |
B1 | 0.0143 (11) | 0.0138 (11) | 0.0142 (12) | −0.0040 (9) | −0.0009 (9) | −0.0019 (9) |
C9 | 0.0122 (9) | 0.0127 (10) | 0.0164 (11) | 0.0011 (8) | 0.0000 (8) | −0.0044 (8) |
C10 | 0.0195 (11) | 0.0161 (11) | 0.0190 (12) | −0.0045 (9) | −0.0003 (9) | −0.0029 (9) |
C11 | 0.0235 (11) | 0.0232 (12) | 0.0200 (12) | −0.0054 (10) | −0.0060 (9) | −0.0075 (10) |
C12 | 0.0265 (12) | 0.0221 (12) | 0.0165 (12) | −0.0021 (10) | −0.0037 (9) | −0.0022 (9) |
C13 | 0.0219 (11) | 0.0170 (11) | 0.0197 (12) | −0.0025 (9) | 0.0003 (9) | 0.0004 (9) |
C14 | 0.0152 (10) | 0.0150 (11) | 0.0201 (12) | −0.0028 (8) | −0.0018 (8) | −0.0036 (9) |
C15 | 0.0144 (10) | 0.0137 (10) | 0.0131 (10) | −0.0022 (8) | −0.0051 (8) | 0.0005 (8) |
C16 | 0.0187 (10) | 0.0176 (11) | 0.0174 (11) | −0.0029 (9) | −0.0014 (9) | −0.0037 (9) |
C17 | 0.0261 (12) | 0.0137 (11) | 0.0244 (13) | −0.0030 (9) | −0.0121 (10) | −0.0008 (9) |
C18 | 0.0263 (12) | 0.0240 (12) | 0.0218 (12) | −0.0156 (10) | −0.0109 (10) | 0.0054 (10) |
C19 | 0.0210 (11) | 0.0317 (13) | 0.0166 (12) | −0.0123 (10) | −0.0030 (9) | −0.0007 (10) |
C20 | 0.0158 (10) | 0.0196 (11) | 0.0171 (11) | −0.0058 (9) | −0.0020 (8) | −0.0035 (9) |
C21 | 0.0152 (10) | 0.0141 (10) | 0.0153 (11) | −0.0064 (8) | 0.0008 (8) | −0.0015 (8) |
C22 | 0.0171 (10) | 0.0184 (11) | 0.0176 (11) | −0.0052 (9) | 0.0000 (8) | −0.0043 (9) |
C23 | 0.0208 (11) | 0.0142 (11) | 0.0229 (12) | −0.0049 (9) | 0.0051 (9) | −0.0046 (9) |
C24 | 0.0345 (13) | 0.0156 (11) | 0.0166 (12) | −0.0104 (10) | 0.0060 (9) | −0.0050 (9) |
C25 | 0.0310 (13) | 0.0248 (13) | 0.0218 (13) | −0.0148 (10) | −0.0026 (10) | −0.0081 (10) |
C26 | 0.0183 (11) | 0.0223 (12) | 0.0207 (12) | −0.0060 (9) | −0.0009 (9) | −0.0059 (9) |
C27 | 0.0152 (10) | 0.0131 (10) | 0.0176 (11) | −0.0039 (8) | −0.0015 (8) | −0.0038 (8) |
C28 | 0.0150 (10) | 0.0161 (11) | 0.0188 (11) | −0.0040 (8) | −0.0016 (8) | −0.0047 (9) |
C29 | 0.0173 (11) | 0.0186 (11) | 0.0244 (12) | −0.0047 (9) | 0.0021 (9) | −0.0083 (9) |
C30 | 0.0141 (10) | 0.0189 (12) | 0.0348 (14) | −0.0002 (9) | −0.0050 (9) | −0.0046 (10) |
C31 | 0.0221 (12) | 0.0228 (12) | 0.0270 (13) | −0.0025 (10) | −0.0076 (10) | 0.0026 (10) |
C32 | 0.0188 (11) | 0.0222 (12) | 0.0197 (12) | −0.0040 (9) | −0.0008 (9) | −0.0012 (9) |
O7 | 0.0340 (12) | 0.0217 (11) | 0.0604 (16) | −0.0027 (10) | −0.0099 (11) | −0.0142 (10) |
Geometric parameters (Å, º) top
Ru1—Ru1i | 2.2823 (5) | B1—C27 | 1.651 (3) |
Ru1—O1i | 2.0444 (16) | C9—C10 | 1.404 (3) |
Ru1—O2 | 2.0451 (15) | C9—C14 | 1.405 (3) |
Ru1—O5 | 2.2921 (16) | C10—C11 | 1.396 (3) |
Ru1—N1 | 2.0266 (19) | C10—H21 | 0.9500 |
Ru1—N2i | 2.0259 (18) | C11—C12 | 1.382 (4) |
Ru2—Ru2ii | 2.2742 (5) | C11—H22 | 0.9500 |
Ru2—O3ii | 2.0457 (15) | C12—C13 | 1.389 (3) |
Ru2—O4 | 2.0509 (15) | C12—H23 | 0.9500 |
Ru2—O6 | 2.3267 (16) | C13—C14 | 1.385 (3) |
Ru2—N3 | 2.0223 (18) | C13—H24 | 0.9500 |
Ru2—N4ii | 2.0299 (18) | C14—H25 | 0.9500 |
N1—C1 | 1.297 (3) | C15—C20 | 1.403 (3) |
N1—H1 | 0.8800 | C15—C16 | 1.405 (3) |
O1—C1 | 1.298 (3) | C16—C17 | 1.385 (3) |
N2—C3 | 1.301 (3) | C16—H26 | 0.9500 |
N2—H2 | 0.8800 | C17—C18 | 1.388 (4) |
O2—C3 | 1.296 (2) | C17—H27 | 0.9500 |
N3—C5 | 1.306 (3) | C18—C19 | 1.382 (4) |
N3—H3 | 0.8800 | C18—H28 | 0.9500 |
O3—C5 | 1.285 (3) | C19—C20 | 1.397 (3) |
N4—C7 | 1.297 (3) | C19—H29 | 0.9500 |
N4—H4 | 0.8800 | C20—H30 | 0.9500 |
O4—C7 | 1.300 (2) | C21—C26 | 1.397 (3) |
O5—H5 | 0.80 (3) | C21—C22 | 1.408 (3) |
O5—H6 | 0.82 (3) | C22—C23 | 1.390 (3) |
O6—H7 | 0.84 (3) | C22—H31 | 0.9500 |
O6—H8 | 0.85 (4) | C23—C24 | 1.390 (3) |
C1—C2 | 1.496 (3) | C23—H32 | 0.9500 |
C2—H9 | 0.9800 | C24—C25 | 1.389 (3) |
C2—H10 | 0.9800 | C24—H33 | 0.9500 |
C2—H11 | 0.9800 | C25—C26 | 1.400 (3) |
C3—C4 | 1.495 (3) | C25—H34 | 0.9500 |
C4—H12 | 0.9800 | C26—H35 | 0.9500 |
C4—H13 | 0.9800 | C27—C32 | 1.403 (3) |
C4—H14 | 0.9800 | C27—C28 | 1.403 (3) |
C5—C6 | 1.498 (3) | C28—C29 | 1.404 (3) |
C6—H15 | 0.9800 | C28—H36 | 0.9500 |
C6—H16 | 0.9800 | C29—C30 | 1.387 (3) |
C6—H17 | 0.9800 | C29—H37 | 0.9500 |
C7—C8 | 1.498 (3) | C30—C31 | 1.388 (4) |
C8—H18 | 0.9800 | C30—H38 | 0.9500 |
C8—H19 | 0.9800 | C31—C32 | 1.395 (3) |
C8—H20 | 0.9800 | C31—H39 | 0.9500 |
B1—C9 | 1.640 (3) | C32—H40 | 0.9500 |
B1—C21 | 1.643 (3) | O7—H41 | 0.74 (4) |
B1—C15 | 1.649 (3) | O7—H42 | 0.70 (5) |
| | | |
N2i—Ru1—N1 | 90.70 (7) | H18—C8—H19 | 109.5 |
N2i—Ru1—O1i | 90.10 (7) | C7—C8—H20 | 109.5 |
N1—Ru1—O1i | 178.79 (6) | H18—C8—H20 | 109.5 |
N2i—Ru1—O2 | 178.01 (7) | H19—C8—H20 | 109.5 |
N1—Ru1—O2 | 91.02 (7) | C9—B1—C21 | 106.72 (17) |
O1i—Ru1—O2 | 88.17 (6) | C9—B1—C15 | 110.11 (18) |
N2i—Ru1—Ru1i | 87.89 (5) | C21—B1—C15 | 110.96 (18) |
N1—Ru1—Ru1i | 86.95 (5) | C9—B1—C27 | 110.13 (18) |
O1i—Ru1—Ru1i | 92.16 (4) | C21—B1—C27 | 112.88 (18) |
O2—Ru1—Ru1i | 91.19 (4) | C15—B1—C27 | 106.08 (17) |
N2i—Ru1—O5 | 92.34 (7) | C10—C9—C14 | 115.2 (2) |
N1—Ru1—O5 | 91.51 (7) | C10—C9—B1 | 125.6 (2) |
O1i—Ru1—O5 | 89.38 (6) | C14—C9—B1 | 119.17 (19) |
O2—Ru1—O5 | 88.63 (6) | C11—C10—C9 | 122.9 (2) |
Ru1i—Ru1—O5 | 178.45 (5) | C11—C10—H21 | 118.6 |
N3—Ru2—N4ii | 90.04 (7) | C9—C10—H21 | 118.6 |
N3—Ru2—O3ii | 178.57 (6) | C12—C11—C10 | 119.8 (2) |
N4ii—Ru2—O3ii | 91.29 (7) | C12—C11—H22 | 120.1 |
N3—Ru2—O4 | 89.23 (7) | C10—C11—H22 | 120.1 |
N4ii—Ru2—O4 | 179.05 (7) | C11—C12—C13 | 119.2 (2) |
O3ii—Ru2—O4 | 89.44 (6) | C11—C12—H23 | 120.4 |
N3—Ru2—Ru2ii | 88.42 (5) | C13—C12—H23 | 120.4 |
N4ii—Ru2—Ru2ii | 87.66 (5) | C14—C13—C12 | 120.3 (2) |
O3ii—Ru2—Ru2ii | 91.10 (4) | C14—C13—H24 | 119.9 |
O4—Ru2—Ru2ii | 91.72 (4) | C12—C13—H24 | 119.9 |
N3—Ru2—O6 | 96.60 (7) | C13—C14—C9 | 122.7 (2) |
N4ii—Ru2—O6 | 93.83 (7) | C13—C14—H25 | 118.7 |
O3ii—Ru2—O6 | 83.85 (6) | C9—C14—H25 | 118.7 |
O4—Ru2—O6 | 86.84 (6) | C20—C15—C16 | 115.3 (2) |
Ru2ii—Ru2—O6 | 174.76 (5) | C20—C15—B1 | 125.9 (2) |
C1—N1—Ru1 | 123.34 (15) | C16—C15—B1 | 118.83 (19) |
C1—N1—H1 | 118.3 | C17—C16—C15 | 123.2 (2) |
Ru1—N1—H1 | 118.3 | C17—C16—H26 | 118.4 |
C1—O1—Ru1i | 117.14 (13) | C15—C16—H26 | 118.4 |
C3—N2—Ru1i | 122.41 (14) | C16—C17—C18 | 119.8 (2) |
C3—N2—H2 | 118.8 | C16—C17—H27 | 120.1 |
Ru1i—N2—H2 | 118.8 | C18—C17—H27 | 120.1 |
C3—O2—Ru1 | 118.19 (13) | C19—C18—C17 | 119.1 (2) |
C5—N3—Ru2 | 121.24 (15) | C19—C18—H28 | 120.4 |
C5—N3—H3 | 119.4 | C17—C18—H28 | 120.4 |
Ru2—N3—H3 | 119.4 | C18—C19—C20 | 120.3 (2) |
C5—O3—Ru2ii | 117.91 (13) | C18—C19—H29 | 119.8 |
C7—N4—Ru2ii | 122.72 (14) | C20—C19—H29 | 119.8 |
C7—N4—H4 | 118.6 | C19—C20—C15 | 122.2 (2) |
Ru2ii—N4—H4 | 118.6 | C19—C20—H30 | 118.9 |
C7—O4—Ru2 | 117.48 (13) | C15—C20—H30 | 118.9 |
Ru1—O5—H5 | 125 (2) | C26—C21—C22 | 115.0 (2) |
Ru1—O5—H6 | 114 (2) | C26—C21—B1 | 125.65 (19) |
H5—O5—H6 | 103 (3) | C22—C21—B1 | 119.36 (19) |
Ru2—O6—H7 | 120 (2) | C23—C22—C21 | 123.3 (2) |
Ru2—O6—H8 | 105 (2) | C23—C22—H31 | 118.4 |
H7—O6—H8 | 104 (3) | C21—C22—H31 | 118.4 |
N1—C1—O1 | 120.4 (2) | C24—C23—C22 | 120.0 (2) |
N1—C1—C2 | 122.9 (2) | C24—C23—H32 | 120.0 |
O1—C1—C2 | 116.67 (19) | C22—C23—H32 | 120.0 |
C1—C2—H9 | 109.5 | C25—C24—C23 | 118.7 (2) |
C1—C2—H10 | 109.5 | C25—C24—H33 | 120.6 |
H9—C2—H10 | 109.5 | C23—C24—H33 | 120.6 |
C1—C2—H11 | 109.5 | C24—C25—C26 | 120.2 (2) |
H9—C2—H11 | 109.5 | C24—C25—H34 | 119.9 |
H10—C2—H11 | 109.5 | C26—C25—H34 | 119.9 |
O2—C3—N2 | 120.23 (19) | C21—C26—C25 | 122.8 (2) |
O2—C3—C4 | 116.07 (19) | C21—C26—H35 | 118.6 |
N2—C3—C4 | 123.70 (19) | C25—C26—H35 | 118.6 |
C3—C4—H12 | 109.5 | C32—C27—C28 | 115.34 (19) |
C3—C4—H13 | 109.5 | C32—C27—B1 | 120.3 (2) |
H12—C4—H13 | 109.5 | C28—C27—B1 | 124.22 (19) |
C3—C4—H14 | 109.5 | C27—C28—C29 | 122.5 (2) |
H12—C4—H14 | 109.5 | C27—C28—H36 | 118.7 |
H13—C4—H14 | 109.5 | C29—C28—H36 | 118.7 |
O3—C5—N3 | 121.26 (19) | C30—C29—C28 | 120.0 (2) |
O3—C5—C6 | 116.99 (19) | C30—C29—H37 | 120.0 |
N3—C5—C6 | 121.74 (19) | C28—C29—H37 | 120.0 |
C5—C6—H15 | 109.5 | C29—C30—C31 | 119.3 (2) |
C5—C6—H16 | 109.5 | C29—C30—H38 | 120.4 |
H15—C6—H16 | 109.5 | C31—C30—H38 | 120.4 |
C5—C6—H17 | 109.5 | C30—C31—C32 | 119.8 (2) |
H15—C6—H17 | 109.5 | C30—C31—H39 | 120.1 |
H16—C6—H17 | 109.5 | C32—C31—H39 | 120.1 |
N4—C7—O4 | 120.34 (19) | C31—C32—C27 | 123.1 (2) |
N4—C7—C8 | 123.02 (19) | C31—C32—H40 | 118.5 |
O4—C7—C8 | 116.64 (19) | C27—C32—H40 | 118.5 |
C7—C8—H18 | 109.5 | H41—O7—H42 | 107 (5) |
C7—C8—H19 | 109.5 | | |
| | | |
N2i—Ru1—N1—C1 | −86.34 (18) | C10—C9—C14—C13 | 0.3 (3) |
O2—Ru1—N1—C1 | 92.65 (17) | B1—C9—C14—C13 | −179.0 (2) |
Ru1i—Ru1—N1—C1 | 1.51 (17) | C9—B1—C15—C20 | −110.7 (2) |
O5—Ru1—N1—C1 | −178.70 (17) | C21—B1—C15—C20 | 7.2 (3) |
N1—Ru1—O2—C3 | −83.83 (16) | C27—B1—C15—C20 | 130.2 (2) |
O1i—Ru1—O2—C3 | 95.27 (15) | C9—B1—C15—C16 | 70.0 (2) |
Ru1i—Ru1—O2—C3 | 3.15 (15) | C21—B1—C15—C16 | −172.09 (18) |
O5—Ru1—O2—C3 | −175.31 (16) | C27—B1—C15—C16 | −49.2 (2) |
N4ii—Ru2—N3—C5 | 84.89 (17) | C20—C15—C16—C17 | 0.0 (3) |
O4—Ru2—N3—C5 | −94.51 (16) | B1—C15—C16—C17 | 179.4 (2) |
Ru2ii—Ru2—N3—C5 | −2.77 (16) | C15—C16—C17—C18 | −0.4 (3) |
O6—Ru2—N3—C5 | 178.75 (16) | C16—C17—C18—C19 | 0.6 (3) |
N3—Ru2—O4—C7 | 90.74 (15) | C17—C18—C19—C20 | −0.3 (3) |
O3ii—Ru2—O4—C7 | −88.74 (15) | C18—C19—C20—C15 | −0.1 (3) |
Ru2ii—Ru2—O4—C7 | 2.34 (14) | C16—C15—C20—C19 | 0.2 (3) |
O6—Ru2—O4—C7 | −172.61 (15) | B1—C15—C20—C19 | −179.1 (2) |
Ru1—N1—C1—O1 | −1.5 (3) | C9—B1—C21—C26 | −131.0 (2) |
Ru1—N1—C1—C2 | 179.24 (16) | C15—B1—C21—C26 | 109.0 (2) |
Ru1i—O1—C1—N1 | 0.5 (3) | C27—B1—C21—C26 | −9.9 (3) |
Ru1i—O1—C1—C2 | 179.77 (15) | C9—B1—C21—C22 | 50.0 (3) |
Ru1—O2—C3—N2 | −3.1 (3) | C15—B1—C21—C22 | −70.0 (2) |
Ru1—O2—C3—C4 | 176.50 (14) | C27—B1—C21—C22 | 171.10 (19) |
Ru1i—N2—C3—O2 | 1.1 (3) | C26—C21—C22—C23 | −1.6 (3) |
Ru1i—N2—C3—C4 | −178.46 (16) | B1—C21—C22—C23 | 177.5 (2) |
Ru2ii—O3—C5—N3 | −1.6 (3) | C21—C22—C23—C24 | 0.1 (4) |
Ru2ii—O3—C5—C6 | 177.33 (14) | C22—C23—C24—C25 | 0.7 (3) |
Ru2—N3—C5—O3 | 3.2 (3) | C23—C24—C25—C26 | 0.0 (4) |
Ru2—N3—C5—C6 | −175.65 (15) | C22—C21—C26—C25 | 2.3 (3) |
Ru2ii—N4—C7—O4 | 2.7 (3) | B1—C21—C26—C25 | −176.7 (2) |
Ru2ii—N4—C7—C8 | −177.39 (15) | C24—C25—C26—C21 | −1.6 (4) |
Ru2—O4—C7—N4 | −3.4 (3) | C9—B1—C27—C32 | −178.2 (2) |
Ru2—O4—C7—C8 | 176.71 (14) | C21—B1—C27—C32 | 62.6 (3) |
C21—B1—C9—C10 | −123.5 (2) | C15—B1—C27—C32 | −59.1 (3) |
C15—B1—C9—C10 | −3.0 (3) | C9—B1—C27—C28 | −2.8 (3) |
C27—B1—C9—C10 | 113.6 (2) | C21—B1—C27—C28 | −122.0 (2) |
C21—B1—C9—C14 | 55.7 (2) | C15—B1—C27—C28 | 116.3 (2) |
C15—B1—C9—C14 | 176.19 (18) | C32—C27—C28—C29 | 0.1 (3) |
C27—B1—C9—C14 | −67.2 (2) | B1—C27—C28—C29 | −175.5 (2) |
C14—C9—C10—C11 | −0.8 (3) | C27—C28—C29—C30 | −0.8 (4) |
B1—C9—C10—C11 | 178.5 (2) | C28—C29—C30—C31 | 0.5 (4) |
C9—C10—C11—C12 | 0.6 (4) | C29—C30—C31—C32 | 0.5 (4) |
C10—C11—C12—C13 | 0.1 (4) | C30—C31—C32—C27 | −1.3 (4) |
C11—C12—C13—C14 | −0.6 (3) | C28—C27—C32—C31 | 0.9 (3) |
C12—C13—C14—C9 | 0.4 (3) | B1—C27—C32—C31 | 176.7 (2) |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O4 | 0.80 (3) | 2.05 (3) | 2.847 (2) | 174 (3) |
O5—H6···O7 | 0.82 (3) | 1.88 (4) | 2.687 (3) | 166 (3) |
O6—H7···O2 | 0.84 (3) | 1.95 (3) | 2.787 (2) | 170 (3) |
N1—H1···O7 | 0.88 | 2.31 | 3.108 (3) | 151 |
N3—H3···O1i | 0.88 | 2.15 | 3.021 (2) | 172 |
Symmetry code: (i) −x+1, −y+1, −z. |
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