Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270104009333/av1174sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270104009333/av1174Isup2.hkl |
CCDC reference: 245844
Compound (NH4)3[Ru2{CH3C(OH)(PO3)2}2]·2H2O was synthesized according to the literature (Yi et al., 2003). A mixture of (NH4)3[Ru2(hedp)2]·2H2O (0.0634 g, 0.089 mmol), Co(en)3Cl3·3H2O (2.0231 g, 5.1 mmol) and water (10 ml) was stirred at 343 K? for 5 h. The filtration was kept at room temperature for 30 d. Brown column-like single crystals were collected as monophasic material. Analysis calculated for (I): C 15.29, N 13.37%; found: C 14.61, N 12.32%. IR (KBr, cm−1): 3.507 (s, br), 3440 (s, br), 3212 (s, br), 2362 (w), 1612 (m), 1579 (s), 1463 (s), 1365 (m), 1326 (m), 1155 (s), 1057 (s), 963 (s), 903 (s), 815 (m), 776 (w), 583 (s), 487 (s), 439 (m).
All H atoms were positioned geometrically and refined as riding, with Uiso values of 1.2 to 1.5 times Ueq of the parent atom, and C—H distances of 0.96 and 0.97 Å, N—H distances of 0.90 Å, and O—H distances of 0.8200–1.1654 Å.
Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Co(C2H8N2)3]2[Ru2Cl2(C2H4O7P2)2]Cl·3H2O | Z = 2 |
Mr = 1245.01 | F(000) = 1262 |
Triclinic, P1 | Dx = 1.669 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.5166 (16) Å | Cell parameters from 1000 reflections |
b = 15.297 (2) Å | θ = 2.3–19.8° |
c = 15.497 (2) Å | µ = 1.61 mm−1 |
α = 90.788 (3)° | T = 293 K |
β = 91.362 (4)° | Prism, brown |
γ = 96.273 (3)° | 0.3 × 0.2 × 0.2 mm |
V = 2477.2 (6) Å3 |
Bruker SMART APEX CCD area-detector diffractometer | 8573 independent reflections |
Radiation source: sealed tube | 6430 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.047 |
ϕ and ω scans | θmax = 25.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −12→6 |
Tmin = 0.69, Tmax = 0.72 | k = −18→18 |
12440 measured reflections | l = −17→18 |
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)] = 0.041 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.109 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.06P)2] where P = (Fo2 + 2Fc2)/3 |
8573 reflections | (Δ/σ)max = 0.001 |
559 parameters | Δρmax = 0.39 e Å−3 |
0 restraints | Δρmin = −0.37 e Å−3 |
[Co(C2H8N2)3]2[Ru2Cl2(C2H4O7P2)2]Cl·3H2O | γ = 96.273 (3)° |
Mr = 1245.01 | V = 2477.2 (6) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.5166 (16) Å | Mo Kα radiation |
b = 15.297 (2) Å | µ = 1.61 mm−1 |
c = 15.497 (2) Å | T = 293 K |
α = 90.788 (3)° | 0.3 × 0.2 × 0.2 mm |
β = 91.362 (4)° |
Bruker SMART APEX CCD area-detector diffractometer | 8573 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | 6430 reflections with I > 2σ(I) |
Tmin = 0.69, Tmax = 0.72 | Rint = 0.047 |
12440 measured reflections |
R[F2 > 2σ(F2)] = 0.041 | 0 restraints |
wR(F2) = 0.109 | H-atom parameters constrained |
S = 1.09 | Δρmax = 0.39 e Å−3 |
8573 reflections | Δρmin = −0.37 e Å−3 |
559 parameters |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ru1 | 0.49084 (4) | 0.49713 (3) | 1.07563 (2) | 0.04397 (11) | |
Ru2 | 0.97359 (4) | −0.07757 (3) | 0.49578 (2) | 0.04410 (12) | |
Co1 | 0.43294 (6) | 0.76962 (4) | 0.24969 (4) | 0.04687 (17) | |
Co2 | 0.82572 (6) | 0.75827 (4) | 0.76128 (4) | 0.04562 (16) | |
P1 | 0.30511 (12) | 0.36186 (8) | 0.98100 (8) | 0.0440 (3) | |
P2 | 0.25596 (12) | 0.55337 (8) | 0.98565 (8) | 0.0453 (3) | |
P3 | 0.82749 (12) | 0.01841 (8) | 0.36461 (8) | 0.0451 (3) | |
P4 | 0.75459 (12) | 0.01992 (8) | 0.55309 (8) | 0.0453 (3) | |
Cl1 | 0.47227 (12) | 0.49354 (8) | 1.24256 (7) | 0.0475 (3) | |
Cl2 | 0.92162 (12) | −0.24439 (8) | 0.48579 (8) | 0.0494 (3) | |
Cl3 | 0.61973 (12) | −0.03218 (8) | 0.85186 (8) | 0.0496 (3) | |
C1 | 0.1789 (5) | 0.7799 (3) | 0.2730 (3) | 0.0514 (12) | |
H1A | 0.1002 | 0.8025 | 0.2545 | 0.062* | |
H1B | 0.1816 | 0.7806 | 0.3356 | 0.062* | |
C2 | 0.1746 (5) | 0.6795 (3) | 0.2393 (4) | 0.0521 (12) | |
H2A | 0.1153 | 0.6401 | 0.2714 | 0.063* | |
H2B | 0.1536 | 0.6734 | 0.1781 | 0.063* | |
C3 | 0.5849 (5) | 0.6821 (3) | 0.3583 (3) | 0.0520 (12) | |
H3A | 0.6710 | 0.6680 | 0.3712 | 0.062* | |
H3B | 0.5256 | 0.6321 | 0.3738 | 0.062* | |
C4 | 0.5595 (5) | 0.7607 (3) | 0.4104 (3) | 0.0476 (11) | |
H4A | 0.5492 | 0.7457 | 0.4706 | 0.057* | |
H4B | 0.6294 | 0.8073 | 0.4062 | 0.057* | |
C5 | 0.6007 (5) | 0.8719 (3) | 0.1428 (3) | 0.0485 (11) | |
H5A | 0.6707 | 0.8355 | 0.1449 | 0.058* | |
H5B | 0.6334 | 0.9298 | 0.1231 | 0.058* | |
C6 | 0.4946 (5) | 0.8307 (3) | 0.0811 (3) | 0.0467 (11) | |
H6A | 0.5303 | 0.8143 | 0.0269 | 0.056* | |
H6B | 0.4332 | 0.8723 | 0.0694 | 0.056* | |
C7 | 0.5999 (5) | 0.7807 (3) | 0.6684 (3) | 0.0474 (11) | |
H7A | 0.5385 | 0.7568 | 0.6242 | 0.057* | |
H7B | 0.6049 | 0.8443 | 0.6673 | 0.057* | |
C8 | 0.5581 (5) | 0.7482 (3) | 0.7558 (3) | 0.0468 (11) | |
H8A | 0.4854 | 0.7772 | 0.7739 | 0.056* | |
H8B | 0.5325 | 0.6854 | 0.7528 | 0.056* | |
C9 | 0.9128 (5) | 0.5892 (3) | 0.7509 (3) | 0.0509 (12) | |
H9A | 0.8876 | 0.5302 | 0.7283 | 0.061* | |
H9B | 0.9763 | 0.5870 | 0.7970 | 0.061* | |
C10 | 0.9602 (5) | 0.6511 (3) | 0.6809 (3) | 0.0521 (12) | |
H10A | 1.0424 | 0.6347 | 0.6634 | 0.063* | |
H10B | 0.9019 | 0.6401 | 0.6315 | 0.063* | |
C11 | 0.9183 (5) | 0.8691 (3) | 0.8963 (3) | 0.0519 (12) | |
H11A | 0.9838 | 0.8842 | 0.9408 | 0.062* | |
H11B | 0.8365 | 0.8808 | 0.9188 | 0.062* | |
C12 | 0.9476 (5) | 0.9232 (3) | 0.8174 (3) | 0.0474 (11) | |
H12A | 0.9352 | 0.9843 | 0.8282 | 0.057* | |
H12B | 1.0351 | 0.9201 | 0.8003 | 0.057* | |
C13 | 0.1837 (5) | 0.4374 (3) | 0.9749 (3) | 0.0442 (11) | |
C14 | 0.1113 (5) | 0.4237 (3) | 0.8875 (3) | 0.0467 (11) | |
H14A | 0.0475 | 0.4639 | 0.8834 | 0.070* | |
H14B | 0.0708 | 0.3644 | 0.8830 | 0.070* | |
H14C | 0.1704 | 0.4343 | 0.8416 | 0.070* | |
C15 | 0.7018 (4) | 0.0301 (3) | 0.4396 (3) | 0.0430 (10) | |
C16 | 0.6551 (5) | 0.1227 (3) | 0.4294 (3) | 0.0478 (11) | |
H16A | 0.5885 | 0.1295 | 0.4695 | 0.072* | |
H16B | 0.6226 | 0.1285 | 0.3716 | 0.072* | |
H16C | 0.7253 | 0.1672 | 0.4409 | 0.072* | |
N1 | 0.2825 (4) | 0.8367 (3) | 0.2442 (3) | 0.0503 (10) | |
H1C | 0.2956 | 0.8851 | 0.2783 | 0.060* | |
H1D | 0.2676 | 0.8534 | 0.1897 | 0.060* | |
N2 | 0.3138 (4) | 0.6654 (3) | 0.2594 (3) | 0.0485 (9) | |
H2C | 0.3367 | 0.6237 | 0.2231 | 0.058* | |
H2D | 0.3195 | 0.6451 | 0.3134 | 0.058* | |
N3 | 0.5711 (4) | 0.6977 (3) | 0.2672 (2) | 0.0470 (9) | |
H3C | 0.5537 | 0.6462 | 0.2382 | 0.056* | |
H3D | 0.6443 | 0.7254 | 0.2473 | 0.056* | |
N4 | 0.4446 (4) | 0.7874 (3) | 0.3747 (3) | 0.0498 (10) | |
H4C | 0.4412 | 0.8447 | 0.3873 | 0.060* | |
H4D | 0.3772 | 0.7565 | 0.3988 | 0.060* | |
N5 | 0.5462 (4) | 0.8788 (3) | 0.2299 (3) | 0.0478 (9) | |
H5C | 0.5014 | 0.9257 | 0.2328 | 0.057* | |
H5D | 0.6094 | 0.8857 | 0.2704 | 0.057* | |
N6 | 0.4293 (4) | 0.7490 (3) | 0.1252 (2) | 0.0474 (9) | |
H6C | 0.4703 | 0.7020 | 0.1128 | 0.057* | |
H6D | 0.3477 | 0.7379 | 0.1057 | 0.057* | |
N7 | 0.7272 (4) | 0.7517 (3) | 0.6517 (2) | 0.0448 (9) | |
H7C | 0.7681 | 0.7868 | 0.6126 | 0.054* | |
H7D | 0.7182 | 0.6962 | 0.6306 | 0.054* | |
N8 | 0.6632 (4) | 0.7671 (3) | 0.8173 (3) | 0.0473 (9) | |
H8C | 0.6545 | 0.7288 | 0.8608 | 0.057* | |
H8D | 0.6622 | 0.8217 | 0.8395 | 0.057* | |
N9 | 0.8032 (4) | 0.6311 (2) | 0.7792 (3) | 0.0460 (9) | |
H9C | 0.7915 | 0.6207 | 0.8356 | 0.055* | |
H9D | 0.7327 | 0.6073 | 0.7498 | 0.055* | |
N10 | 0.9752 (4) | 0.7415 (3) | 0.6970 (3) | 0.0489 (10) | |
H10C | 0.9770 | 0.7717 | 0.6476 | 0.059* | |
H10D | 1.0473 | 0.7580 | 0.7283 | 0.059* | |
N11 | 0.9146 (4) | 0.7781 (2) | 0.8728 (2) | 0.0469 (9) | |
H11C | 0.8734 | 0.7447 | 0.9130 | 0.056* | |
H11D | 0.9947 | 0.7630 | 0.8695 | 0.056* | |
N12 | 0.8596 (4) | 0.8853 (2) | 0.7524 (2) | 0.0459 (9) | |
H12C | 0.8913 | 0.8984 | 0.7001 | 0.055* | |
H12D | 0.7855 | 0.9092 | 0.7566 | 0.055* | |
O1 | 0.2443 (3) | 0.2700 (2) | 0.9768 (2) | 0.0467 (8) | |
O2 | 0.4029 (3) | 0.3828 (2) | 0.9087 (2) | 0.0465 (8) | |
O3 | 0.3770 (3) | 0.3822 (2) | 1.0689 (2) | 0.0446 (7) | |
O4 | 0.3540 (3) | 0.5671 (2) | 0.9129 (2) | 0.0456 (7) | |
O5 | 0.1528 (3) | 0.6123 (2) | 0.9793 (2) | 0.0455 (7) | |
O6 | 0.3296 (3) | 0.5609 (2) | 1.0742 (2) | 0.0472 (8) | |
O7 | 0.1046 (3) | 0.4190 (2) | 1.0471 (2) | 0.0451 (7) | |
H7E | 0.0295 | 0.4107 | 1.0306 | 0.054* | |
O8 | 0.9355 (3) | 0.0916 (2) | 0.3890 (2) | 0.0459 (7) | |
O9 | 0.8769 (3) | −0.0708 (2) | 0.3834 (2) | 0.0454 (7) | |
O10 | 0.7762 (3) | 0.0220 (2) | 0.2755 (2) | 0.0473 (8) | |
O11 | 0.6505 (3) | 0.0295 (2) | 0.6139 (2) | 0.0469 (8) | |
O12 | 0.8075 (3) | −0.0695 (2) | 0.5574 (2) | 0.0463 (7) | |
O13 | 0.8665 (3) | 0.0922 (2) | 0.5673 (2) | 0.0452 (7) | |
O14 | 0.5989 (3) | −0.0386 (2) | 0.4190 (2) | 0.0489 (8) | |
H14D | 0.5318 | −0.0167 | 0.4117 | 0.059* | |
O1W | 0.6641 (3) | 0.1073 (2) | 0.1513 (2) | 0.0517 (8) | |
H1WA | 0.7161 | 0.0799 | 0.1804 | 0.062* | |
H1WB | 0.5880 | 0.0906 | 0.1659 | 0.062* | |
O2W | 0.2669 (11) | 0.5831 (8) | 0.7125 (8) | 0.046 (3) | 0.25 |
H2WB | 0.2091 | 0.5466 | 0.6891 | 0.055* | 0.25 |
H2WD | 0.3367 | 0.5815 | 0.6863 | 0.055* | 0.25 |
O3W | 0.1810 (12) | 0.7250 (8) | 0.8344 (7) | 0.043 (3) | 0.25 |
H3WD | 0.1987 | 0.6843 | 0.8004 | 0.052* | 0.25 |
H3WC | 0.2499 | 0.7518 | 0.8558 | 0.052* | 0.25 |
O4W | 0.8691 (13) | 0.8099 (10) | 0.2777 (9) | 0.057 (4) | 0.25 |
H4WA | 0.8847 | 0.8338 | 0.2294 | 0.068* | 0.25 |
H4WC | 0.8789 | 0.8486 | 0.3179 | 0.068* | 0.25 |
O5W | 0.1730 (12) | 0.7850 (8) | 0.0536 (8) | 0.046 (3) | 0.25 |
H5WB | 0.0947 | 0.7691 | 0.0412 | 0.055* | 0.25 |
H5WC | 0.1880 | 0.8405 | 0.0493 | 0.055* | 0.25 |
O6W | 0.0679 (12) | 0.1600 (7) | 0.8929 (8) | 0.043 (3) | 0.25 |
H6WA | 0.0627 | 0.1107 | 0.9178 | 0.064* | 0.25 |
H6WC | 0.0948 | 0.1542 | 0.8420 | 0.064* | 0.25 |
O7W | 0.9456 (13) | 0.5207 (9) | 0.4205 (9) | 0.054 (3) | 0.25 |
H7WB | 1.0045 | 0.4880 | 0.4119 | 0.065* | 0.25 |
H7WD | 0.8916 | 0.5023 | 0.4578 | 0.065* | 0.25 |
O8W | 0.3120 (12) | 0.6189 (9) | 0.4856 (8) | 0.049 (3) | 0.25 |
H8WD | 0.3923 | 0.6233 | 0.4784 | 0.059* | 0.25 |
H8WA | 0.3051 | 0.5983 | 0.5576 | 0.059* | 0.25 |
O9W | 0.6361 (13) | 0.5715 (8) | 0.5703 (7) | 0.045 (3) | 0.25 |
H9WA | 0.6254 | 0.5584 | 0.5169 | 0.054* | 0.25 |
H9WD | 0.5868 | 0.5365 | 0.5998 | 0.054* | 0.25 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru1 | 0.0434 (2) | 0.0438 (2) | 0.0446 (2) | 0.00423 (17) | 0.00133 (16) | 0.00031 (16) |
Ru2 | 0.0435 (2) | 0.0444 (2) | 0.0443 (2) | 0.00456 (17) | 0.00169 (16) | 0.00038 (16) |
Co1 | 0.0457 (4) | 0.0463 (4) | 0.0484 (4) | 0.0043 (3) | 0.0015 (3) | −0.0008 (3) |
Co2 | 0.0456 (4) | 0.0456 (4) | 0.0458 (4) | 0.0047 (3) | 0.0022 (3) | 0.0035 (3) |
P1 | 0.0417 (6) | 0.0447 (7) | 0.0452 (7) | 0.0037 (5) | −0.0001 (5) | 0.0007 (5) |
P2 | 0.0443 (7) | 0.0451 (7) | 0.0465 (7) | 0.0049 (5) | −0.0004 (5) | 0.0017 (5) |
P3 | 0.0447 (7) | 0.0458 (7) | 0.0446 (7) | 0.0046 (5) | 0.0003 (5) | 0.0001 (5) |
P4 | 0.0439 (7) | 0.0471 (7) | 0.0449 (7) | 0.0049 (5) | 0.0020 (5) | 0.0011 (5) |
Cl1 | 0.0505 (7) | 0.0455 (6) | 0.0461 (6) | 0.0033 (5) | 0.0022 (5) | 0.0008 (5) |
Cl2 | 0.0512 (7) | 0.0481 (6) | 0.0488 (6) | 0.0052 (5) | 0.0002 (5) | −0.0006 (5) |
Cl3 | 0.0492 (7) | 0.0473 (6) | 0.0527 (7) | 0.0070 (5) | 0.0005 (5) | 0.0006 (5) |
C1 | 0.051 (3) | 0.043 (3) | 0.059 (3) | 0.001 (2) | 0.001 (2) | 0.001 (2) |
C2 | 0.048 (3) | 0.046 (3) | 0.062 (3) | 0.003 (2) | −0.003 (2) | −0.003 (2) |
C3 | 0.051 (3) | 0.048 (3) | 0.057 (3) | 0.005 (2) | 0.002 (2) | −0.003 (2) |
C4 | 0.050 (3) | 0.051 (3) | 0.042 (3) | 0.005 (2) | 0.000 (2) | −0.005 (2) |
C5 | 0.047 (3) | 0.050 (3) | 0.049 (3) | 0.008 (2) | 0.001 (2) | 0.001 (2) |
C6 | 0.050 (3) | 0.045 (3) | 0.046 (3) | 0.007 (2) | 0.007 (2) | 0.002 (2) |
C7 | 0.048 (3) | 0.046 (3) | 0.047 (3) | −0.001 (2) | 0.006 (2) | 0.001 (2) |
C8 | 0.044 (3) | 0.051 (3) | 0.045 (3) | 0.006 (2) | 0.001 (2) | −0.004 (2) |
C9 | 0.057 (3) | 0.046 (3) | 0.052 (3) | 0.014 (2) | −0.003 (2) | 0.004 (2) |
C10 | 0.052 (3) | 0.050 (3) | 0.053 (3) | 0.005 (2) | −0.002 (2) | −0.002 (2) |
C11 | 0.049 (3) | 0.053 (3) | 0.052 (3) | −0.003 (2) | 0.005 (2) | 0.004 (2) |
C12 | 0.043 (3) | 0.053 (3) | 0.046 (3) | 0.005 (2) | 0.007 (2) | 0.003 (2) |
C13 | 0.053 (3) | 0.039 (2) | 0.041 (2) | 0.009 (2) | 0.001 (2) | −0.0041 (19) |
C14 | 0.045 (3) | 0.041 (2) | 0.053 (3) | 0.002 (2) | 0.000 (2) | 0.003 (2) |
C15 | 0.036 (2) | 0.057 (3) | 0.036 (2) | 0.002 (2) | −0.0003 (19) | 0.004 (2) |
C16 | 0.050 (3) | 0.047 (3) | 0.046 (3) | 0.004 (2) | 0.000 (2) | 0.006 (2) |
N1 | 0.053 (2) | 0.047 (2) | 0.051 (2) | 0.0044 (19) | −0.0012 (19) | −0.0022 (18) |
N2 | 0.046 (2) | 0.043 (2) | 0.057 (2) | 0.0014 (18) | 0.0031 (19) | −0.0007 (18) |
N3 | 0.049 (2) | 0.046 (2) | 0.046 (2) | 0.0059 (18) | 0.0014 (18) | −0.0022 (17) |
N4 | 0.051 (2) | 0.043 (2) | 0.055 (2) | 0.0026 (19) | 0.0055 (19) | −0.0003 (18) |
N5 | 0.045 (2) | 0.047 (2) | 0.050 (2) | 0.0020 (18) | 0.0009 (18) | −0.0029 (18) |
N6 | 0.047 (2) | 0.050 (2) | 0.045 (2) | 0.0066 (19) | −0.0025 (18) | −0.0020 (18) |
N7 | 0.044 (2) | 0.044 (2) | 0.047 (2) | 0.0068 (18) | −0.0020 (18) | 0.0005 (17) |
N8 | 0.047 (2) | 0.048 (2) | 0.048 (2) | 0.0071 (18) | 0.0059 (18) | 0.0006 (18) |
N9 | 0.047 (2) | 0.046 (2) | 0.045 (2) | 0.0047 (18) | 0.0017 (18) | 0.0024 (17) |
N10 | 0.047 (2) | 0.050 (2) | 0.050 (2) | 0.0068 (19) | 0.0003 (19) | 0.0007 (18) |
N11 | 0.049 (2) | 0.044 (2) | 0.048 (2) | 0.0074 (18) | −0.0055 (18) | 0.0029 (17) |
N12 | 0.052 (2) | 0.040 (2) | 0.046 (2) | 0.0016 (18) | 0.0061 (18) | 0.0015 (17) |
O1 | 0.0466 (18) | 0.0440 (18) | 0.0499 (19) | 0.0062 (15) | 0.0034 (15) | −0.0032 (14) |
O2 | 0.054 (2) | 0.0412 (17) | 0.0435 (18) | 0.0020 (15) | −0.0003 (15) | −0.0031 (14) |
O3 | 0.0446 (18) | 0.0442 (18) | 0.0449 (17) | 0.0044 (14) | −0.0007 (14) | 0.0019 (14) |
O4 | 0.0464 (18) | 0.0426 (17) | 0.0485 (18) | 0.0072 (14) | 0.0015 (15) | 0.0037 (14) |
O5 | 0.0451 (18) | 0.0478 (18) | 0.0432 (17) | 0.0027 (15) | 0.0025 (14) | 0.0044 (14) |
O6 | 0.0450 (18) | 0.0492 (18) | 0.0482 (18) | 0.0083 (15) | 0.0033 (15) | 0.0020 (14) |
O7 | 0.0399 (17) | 0.0479 (18) | 0.0477 (18) | 0.0059 (14) | 0.0003 (14) | 0.0013 (14) |
O8 | 0.0458 (18) | 0.0473 (18) | 0.0451 (18) | 0.0076 (15) | 0.0009 (15) | −0.0005 (14) |
O9 | 0.0469 (18) | 0.0459 (18) | 0.0435 (17) | 0.0049 (15) | 0.0013 (14) | −0.0021 (14) |
O10 | 0.0499 (19) | 0.0469 (18) | 0.0448 (18) | 0.0044 (15) | −0.0017 (15) | 0.0001 (14) |
O11 | 0.0429 (18) | 0.0476 (18) | 0.0494 (19) | 0.0003 (15) | 0.0058 (15) | −0.0010 (14) |
O12 | 0.0411 (18) | 0.0512 (19) | 0.0464 (18) | 0.0054 (15) | −0.0007 (14) | −0.0027 (14) |
O13 | 0.0415 (17) | 0.0465 (18) | 0.0485 (18) | 0.0093 (14) | 0.0019 (14) | −0.0018 (14) |
O14 | 0.0431 (18) | 0.0529 (19) | 0.0499 (19) | 0.0031 (15) | −0.0040 (15) | −0.0027 (15) |
O1W | 0.053 (2) | 0.053 (2) | 0.0496 (19) | 0.0105 (16) | 0.0005 (16) | 0.0014 (15) |
O2W | 0.031 (6) | 0.053 (8) | 0.054 (8) | 0.010 (6) | 0.009 (6) | 0.008 (6) |
O3W | 0.053 (8) | 0.045 (7) | 0.030 (6) | 0.002 (6) | −0.013 (5) | 0.013 (5) |
O4W | 0.046 (8) | 0.072 (9) | 0.057 (8) | 0.032 (7) | −0.002 (6) | 0.011 (7) |
O5W | 0.043 (7) | 0.041 (7) | 0.053 (8) | 0.003 (6) | 0.013 (6) | 0.006 (6) |
O6W | 0.050 (7) | 0.031 (6) | 0.045 (7) | −0.008 (5) | −0.013 (6) | 0.007 (5) |
O7W | 0.055 (8) | 0.051 (8) | 0.059 (8) | 0.016 (7) | 0.010 (7) | 0.013 (6) |
O8W | 0.036 (7) | 0.062 (8) | 0.053 (8) | 0.015 (6) | 0.017 (6) | 0.008 (6) |
O9W | 0.061 (8) | 0.044 (7) | 0.032 (6) | 0.012 (6) | 0.002 (6) | 0.006 (5) |
Ru1—O4i | 2.000 (3) | C9—H9A | 0.9700 |
Ru1—O3 | 2.015 (3) | C9—H9B | 0.9700 |
Ru1—O6 | 2.047 (3) | C10—N10 | 1.393 (6) |
Ru1—O2i | 2.051 (3) | C10—H10A | 0.9700 |
Ru1—Ru1i | 2.3587 (8) | C10—H10B | 0.9700 |
Ru1—Cl1 | 2.5997 (13) | C11—N11 | 1.430 (6) |
Ru2—O13ii | 1.997 (3) | C11—C12 | 1.505 (7) |
Ru2—O9 | 2.005 (3) | C11—H11A | 0.9700 |
Ru2—O12 | 2.025 (3) | C11—H11B | 0.9700 |
Ru2—O8ii | 2.031 (3) | C12—N12 | 1.425 (6) |
Ru2—Ru2ii | 2.3785 (8) | C12—H12A | 0.9700 |
Ru2—Cl2 | 2.5525 (13) | C12—H12B | 0.9700 |
Co1—N2 | 1.927 (4) | C13—O7 | 1.422 (6) |
Co1—N3 | 1.932 (4) | C13—C14 | 1.539 (6) |
Co1—N6 | 1.949 (4) | C14—H14A | 0.9600 |
Co1—N4 | 1.951 (4) | C14—H14B | 0.9600 |
Co1—N5 | 1.975 (4) | C14—H14C | 0.9600 |
Co1—N1 | 1.979 (4) | C15—O14 | 1.450 (5) |
Co2—N10 | 1.920 (4) | C15—C16 | 1.558 (6) |
Co2—N12 | 1.945 (4) | C16—H16A | 0.9600 |
Co2—N11 | 1.949 (4) | C16—H16B | 0.9600 |
Co2—N8 | 1.952 (4) | C16—H16C | 0.9600 |
Co2—N9 | 1.958 (4) | N1—H1C | 0.9000 |
Co2—N7 | 1.964 (4) | N1—H1D | 0.9000 |
P1—O1 | 1.479 (3) | N2—H2C | 0.9000 |
P1—O2 | 1.552 (4) | N2—H2D | 0.9000 |
P1—O3 | 1.554 (3) | N3—H3C | 0.9000 |
P1—C13 | 1.815 (5) | N3—H3D | 0.9000 |
P2—O5 | 1.487 (3) | N4—H4C | 0.9000 |
P2—O4 | 1.547 (4) | N4—H4D | 0.9000 |
P2—O6 | 1.556 (3) | N5—H5C | 0.9000 |
P2—C13 | 1.855 (5) | N5—H5D | 0.9000 |
P3—O10 | 1.475 (3) | N6—H6C | 0.9000 |
P3—O9 | 1.541 (3) | N6—H6D | 0.9000 |
P3—O8 | 1.542 (3) | N7—H7C | 0.9000 |
P3—C15 | 1.803 (5) | N7—H7D | 0.9000 |
P4—O11 | 1.479 (3) | N8—H8C | 0.9000 |
P4—O12 | 1.533 (3) | N8—H8D | 0.9000 |
P4—O13 | 1.534 (3) | N9—H9C | 0.9000 |
P4—C15 | 1.845 (4) | N9—H9D | 0.9000 |
C1—N1 | 1.403 (6) | N10—H10C | 0.9000 |
C1—C2 | 1.611 (7) | N10—H10D | 0.9000 |
C1—H1A | 0.9700 | N11—H11C | 0.9000 |
C1—H1B | 0.9700 | N11—H11D | 0.9000 |
C2—N2 | 1.528 (6) | N12—H12C | 0.9000 |
C2—H2A | 0.9700 | N12—H12D | 0.9000 |
C2—H2B | 0.9700 | O2—Ru1i | 2.051 (3) |
C3—N3 | 1.442 (6) | O4—Ru1i | 2.000 (3) |
C3—C4 | 1.491 (6) | O7—H7E | 0.8200 |
C3—H3A | 0.9700 | O8—Ru2ii | 2.031 (3) |
C3—H3B | 0.9701 | O13—Ru2ii | 1.997 (3) |
C4—N4 | 1.420 (6) | O14—H14D | 0.8200 |
C4—H4A | 0.9700 | O1W—H1WA | 0.8498 |
C4—H4B | 0.9700 | O1W—H1WB | 0.8500 |
C5—N5 | 1.485 (6) | O2W—H2WB | 0.8499 |
C5—C6 | 1.528 (7) | O2W—H2WD | 0.8500 |
C5—H5A | 0.9700 | O3W—H3WD | 0.8499 |
C5—H5B | 0.9700 | O3W—H3WC | 0.8501 |
C6—N6 | 1.537 (6) | O4W—H4WA | 0.8501 |
C6—H6A | 0.9700 | O4W—H4WC | 0.8496 |
C6—H6B | 0.9700 | O5W—H5WB | 0.8500 |
C7—N7 | 1.482 (6) | O5W—H5WC | 0.8501 |
C7—C8 | 1.507 (7) | O6W—H6WA | 0.8501 |
C7—H7A | 0.9700 | O6W—H6WC | 0.8501 |
C7—H7B | 0.9700 | O7W—H7WB | 0.8500 |
C8—N8 | 1.444 (6) | O7W—H7WD | 0.8501 |
C8—H8A | 0.9700 | O8W—H8WD | 0.8500 |
C8—H8B | 0.9700 | O8W—H8WA | 1.1654 |
C9—N9 | 1.452 (6) | O9W—H9WA | 0.8499 |
C9—C10 | 1.508 (7) | O9W—H9WD | 0.8500 |
O4i—Ru1—O3 | 90.69 (13) | C10—C9—H9B | 111.7 |
O4i—Ru1—O6 | 175.38 (13) | H9A—C9—H9B | 109.5 |
O3—Ru1—O6 | 88.41 (13) | N10—C10—C9 | 119.8 (4) |
O4i—Ru1—O2i | 92.24 (13) | N10—C10—H10A | 107.4 |
O3—Ru1—O2i | 174.93 (13) | C9—C10—H10A | 107.4 |
O6—Ru1—O2i | 88.34 (13) | N10—C10—H10B | 107.4 |
O4i—Ru1—Ru1i | 91.52 (9) | C9—C10—H10B | 107.4 |
O3—Ru1—Ru1i | 92.61 (9) | H10A—C10—H10B | 106.9 |
O6—Ru1—Ru1i | 93.05 (9) | N11—C11—C12 | 108.6 (4) |
O2i—Ru1—Ru1i | 91.45 (9) | N11—C11—H11A | 110.0 |
O4i—Ru1—Cl1 | 88.69 (10) | C12—C11—H11A | 110.0 |
O3—Ru1—Cl1 | 88.33 (9) | N11—C11—H11B | 110.0 |
O6—Ru1—Cl1 | 86.75 (9) | C12—C11—H11B | 110.0 |
O2i—Ru1—Cl1 | 87.60 (9) | H11A—C11—H11B | 108.3 |
Ru1i—Ru1—Cl1 | 179.04 (4) | N12—C12—C11 | 104.9 (4) |
O13ii—Ru2—O9 | 90.48 (13) | N12—C12—H12A | 110.8 |
O13ii—Ru2—O12 | 176.82 (12) | C11—C12—H12A | 110.8 |
O9—Ru2—O12 | 88.42 (13) | N12—C12—H12B | 110.8 |
O13ii—Ru2—O8ii | 91.02 (13) | C11—C12—H12B | 110.8 |
O9—Ru2—O8ii | 176.38 (13) | H12A—C12—H12B | 108.8 |
O12—Ru2—O8ii | 89.92 (13) | O7—C13—C14 | 113.5 (4) |
O13ii—Ru2—Ru2ii | 91.29 (9) | O7—C13—P1 | 106.0 (3) |
O9—Ru2—Ru2ii | 92.48 (9) | C14—C13—P1 | 108.8 (3) |
O12—Ru2—Ru2ii | 91.74 (9) | O7—C13—P2 | 107.8 (3) |
O8ii—Ru2—Ru2ii | 90.78 (9) | C14—C13—P2 | 109.4 (3) |
O13ii—Ru2—Cl2 | 87.55 (10) | P1—C13—P2 | 111.3 (3) |
O9—Ru2—Cl2 | 87.80 (9) | C13—C14—H14A | 109.5 |
O12—Ru2—Cl2 | 89.42 (10) | C13—C14—H14B | 109.5 |
O8ii—Ru2—Cl2 | 88.97 (9) | H14A—C14—H14B | 109.5 |
Ru2ii—Ru2—Cl2 | 178.81 (4) | C13—C14—H14C | 109.5 |
N2—Co1—N3 | 88.64 (17) | H14A—C14—H14C | 109.5 |
N2—Co1—N6 | 88.29 (17) | H14B—C14—H14C | 109.5 |
N3—Co1—N6 | 92.25 (16) | O14—C15—C16 | 110.7 (4) |
N2—Co1—N4 | 92.12 (18) | O14—C15—P3 | 107.3 (3) |
N3—Co1—N4 | 84.89 (16) | C16—C15—P3 | 109.1 (3) |
N6—Co1—N4 | 177.09 (18) | O14—C15—P4 | 109.2 (3) |
N2—Co1—N5 | 174.68 (17) | C16—C15—P4 | 107.8 (3) |
N3—Co1—N5 | 94.83 (18) | P3—C15—P4 | 112.8 (2) |
N6—Co1—N5 | 87.54 (17) | C15—C16—H16A | 109.5 |
N4—Co1—N5 | 92.21 (17) | C15—C16—H16B | 109.5 |
N2—Co1—N1 | 87.05 (17) | H16A—C16—H16B | 109.5 |
N3—Co1—N1 | 173.20 (17) | C15—C16—H16C | 109.5 |
N6—Co1—N1 | 92.88 (17) | H16A—C16—H16C | 109.5 |
N4—Co1—N1 | 90.01 (17) | H16B—C16—H16C | 109.5 |
N5—Co1—N1 | 89.85 (17) | C1—N1—Co1 | 106.2 (3) |
N10—Co2—N12 | 91.33 (17) | C1—N1—H1C | 110.5 |
N10—Co2—N11 | 95.94 (18) | Co1—N1—H1C | 110.5 |
N12—Co2—N11 | 83.70 (16) | C1—N1—H1D | 110.5 |
N10—Co2—N8 | 173.79 (17) | Co1—N1—H1D | 110.5 |
N12—Co2—N8 | 92.16 (17) | H1C—N1—H1D | 108.7 |
N11—Co2—N8 | 89.55 (17) | C2—N2—Co1 | 114.2 (3) |
N10—Co2—N9 | 87.89 (17) | C2—N2—H2C | 108.7 |
N12—Co2—N9 | 174.68 (17) | Co1—N2—H2C | 108.7 |
N11—Co2—N9 | 91.15 (16) | C2—N2—H2D | 108.7 |
N8—Co2—N9 | 89.10 (17) | Co1—N2—H2D | 108.7 |
N10—Co2—N7 | 88.38 (17) | H2C—N2—H2D | 107.6 |
N12—Co2—N7 | 90.73 (16) | C3—N3—Co1 | 108.5 (3) |
N11—Co2—N7 | 173.01 (16) | C3—N3—H3C | 110.0 |
N8—Co2—N7 | 86.44 (17) | Co1—N3—H3C | 110.0 |
N9—Co2—N7 | 94.51 (16) | C3—N3—H3D | 110.0 |
O1—P1—O2 | 112.85 (18) | Co1—N3—H3D | 110.0 |
O1—P1—O3 | 111.01 (18) | H3C—N3—H3D | 108.4 |
O2—P1—O3 | 107.50 (18) | C4—N4—Co1 | 111.9 (3) |
O1—P1—C13 | 110.1 (2) | C4—N4—H4C | 109.2 |
O2—P1—C13 | 109.4 (2) | Co1—N4—H4C | 109.2 |
O3—P1—C13 | 105.71 (19) | C4—N4—H4D | 109.2 |
O5—P2—O4 | 113.25 (18) | Co1—N4—H4D | 109.2 |
O5—P2—O6 | 113.20 (18) | H4C—N4—H4D | 107.9 |
O4—P2—O6 | 108.69 (19) | C5—N5—Co1 | 107.9 (3) |
O5—P2—C13 | 109.1 (2) | C5—N5—H5C | 110.1 |
O4—P2—C13 | 106.1 (2) | Co1—N5—H5C | 110.1 |
O6—P2—C13 | 106.1 (2) | C5—N5—H5D | 110.1 |
O10—P3—O9 | 111.89 (18) | Co1—N5—H5D | 110.1 |
O10—P3—O8 | 114.68 (19) | H5C—N5—H5D | 108.4 |
O9—P3—O8 | 107.95 (18) | C6—N6—Co1 | 109.3 (3) |
O10—P3—C15 | 109.6 (2) | C6—N6—H6C | 109.8 |
O9—P3—C15 | 106.4 (2) | Co1—N6—H6C | 109.8 |
O8—P3—C15 | 105.9 (2) | C6—N6—H6D | 109.8 |
O11—P4—O12 | 113.73 (19) | Co1—N6—H6D | 109.8 |
O11—P4—O13 | 111.75 (18) | H6C—N6—H6D | 108.3 |
O12—P4—O13 | 108.25 (18) | C7—N7—Co2 | 108.0 (3) |
O11—P4—C15 | 112.2 (2) | C7—N7—H7C | 110.1 |
O12—P4—C15 | 105.2 (2) | Co2—N7—H7C | 110.1 |
O13—P4—C15 | 105.2 (2) | C7—N7—H7D | 110.1 |
N1—C1—C2 | 115.0 (4) | Co2—N7—H7D | 110.1 |
N1—C1—H1A | 108.5 | H7C—N7—H7D | 108.4 |
C2—C1—H1A | 108.5 | C8—N8—Co2 | 110.2 (3) |
N1—C1—H1B | 108.5 | C8—N8—H8C | 109.6 |
C2—C1—H1B | 108.5 | Co2—N8—H8C | 109.6 |
H1A—C1—H1B | 107.5 | C8—N8—H8D | 109.6 |
N2—C2—C1 | 98.7 (4) | Co2—N8—H8D | 109.6 |
N2—C2—H2A | 112.0 | H8C—N8—H8D | 108.1 |
C1—C2—H2A | 112.0 | C9—N9—Co2 | 111.9 (3) |
N2—C2—H2B | 112.0 | C9—N9—H9C | 109.2 |
C1—C2—H2B | 112.0 | Co2—N9—H9C | 109.2 |
H2A—C2—H2B | 109.7 | C9—N9—H9D | 109.2 |
N3—C3—C4 | 111.1 (4) | Co2—N9—H9D | 109.2 |
N3—C3—H3A | 109.4 | H9C—N9—H9D | 107.9 |
C4—C3—H3A | 109.5 | C10—N10—Co2 | 102.4 (3) |
N3—C3—H3B | 109.3 | C10—N10—H10C | 111.3 |
C4—C3—H3B | 109.5 | Co2—N10—H10C | 111.3 |
H3A—C3—H3B | 107.9 | C10—N10—H10D | 111.3 |
N4—C4—C3 | 105.4 (4) | Co2—N10—H10D | 111.3 |
N4—C4—H4A | 110.7 | H10C—N10—H10D | 109.2 |
C3—C4—H4A | 110.7 | C11—N11—Co2 | 108.8 (3) |
N4—C4—H4B | 110.7 | C11—N11—H11C | 109.9 |
C3—C4—H4B | 110.7 | Co2—N11—H11C | 109.9 |
H4A—C4—H4B | 108.8 | C11—N11—H11D | 109.9 |
N5—C5—C6 | 108.2 (4) | Co2—N11—H11D | 109.9 |
N5—C5—H5A | 110.1 | H11C—N11—H11D | 108.3 |
C6—C5—H5A | 110.1 | C12—N12—Co2 | 112.6 (3) |
N5—C5—H5B | 110.1 | C12—N12—H12C | 109.1 |
C6—C5—H5B | 110.1 | Co2—N12—H12C | 109.1 |
H5A—C5—H5B | 108.4 | C12—N12—H12D | 109.1 |
C5—C6—N6 | 107.1 (4) | Co2—N12—H12D | 109.1 |
C5—C6—H6A | 110.3 | H12C—N12—H12D | 107.8 |
N6—C6—H6A | 110.3 | P1—O2—Ru1i | 113.53 (17) |
C5—C6—H6B | 110.3 | P1—O3—Ru1 | 115.21 (18) |
N6—C6—H6B | 110.3 | P2—O4—Ru1i | 116.35 (18) |
H6A—C6—H6B | 108.5 | P2—O6—Ru1 | 113.17 (18) |
N7—C7—C8 | 108.5 (4) | C13—O7—H7E | 109.5 |
N7—C7—H7A | 110.0 | P3—O8—Ru2ii | 115.45 (19) |
C8—C7—H7A | 110.0 | P3—O9—Ru2 | 115.69 (17) |
N7—C7—H7B | 110.0 | P4—O12—Ru2 | 115.50 (19) |
C8—C7—H7B | 110.0 | P4—O13—Ru2ii | 116.70 (18) |
H7A—C7—H7B | 108.4 | C15—O14—H14D | 109.5 |
N8—C8—C7 | 109.1 (4) | H1WA—O1W—H1WB | 109.5 |
N8—C8—H8A | 109.9 | H2WB—O2W—H2WD | 109.8 |
C7—C8—H8A | 109.9 | H3WD—O3W—H3WC | 109.5 |
N8—C8—H8B | 109.9 | H4WA—O4W—H4WC | 109.8 |
C7—C8—H8B | 109.9 | H5WB—O5W—H5WC | 109.5 |
H8A—C8—H8B | 108.3 | H6WA—O6W—H6WC | 109.5 |
N9—C9—C10 | 100.3 (4) | H7WB—O7W—H7WD | 115.1 |
N9—C9—H9A | 111.7 | H8WD—O8W—H8WA | 101.7 |
C10—C9—H9A | 111.7 | H9WA—O9W—H9WD | 109.8 |
N9—C9—H9B | 111.7 |
Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) −x+2, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O3W—H3WD···O2W | 0.85 | 2.23 | 3.081 (18) | 174 |
O1W—H1WA···O10 | 0.85 | 1.86 | 2.663 (4) | 157 |
N7—H7D···O9W | 0.90 | 2.19 | 3.062 (13) | 162 |
N6—H6D···O5W | 0.90 | 2.19 | 2.999 (14) | 150 |
N1—H1C···O11iii | 0.90 | 2.13 | 3.001 (5) | 162 |
N4—H4C···O11iii | 0.90 | 2.24 | 3.079 (5) | 154 |
N5—H5C···Cl3iii | 0.90 | 2.54 | 3.320 (4) | 146 |
N6—H6C···O2iii | 0.90 | 1.99 | 2.872 (5) | 167 |
O2W—H2WB···O7Wiii | 0.85 | 2.46 | 3.268 (19) | 159 |
O4W—H4WA···O6Wiii | 0.85 | 1.97 | 2.773 (19) | 157 |
O6W—H6WC···O4Wiii | 0.85 | 1.98 | 2.773 (19) | 156 |
N2—H2C···O6iv | 0.90 | 2.48 | 3.282 (5) | 148 |
N3—H3C···Cl1iv | 0.90 | 2.40 | 3.197 (4) | 148 |
N7—H7C···O12v | 0.90 | 2.37 | 3.161 (5) | 147 |
N8—H8D···Cl3v | 0.90 | 2.33 | 3.193 (4) | 160 |
N10—H10C···Cl2v | 0.90 | 2.56 | 3.323 (4) | 143 |
O4W—H4WC···O9v | 0.85 | 1.59 | 2.429 (15) | 169 |
N8—H8C···O3i | 0.90 | 2.03 | 2.906 (5) | 164 |
N9—H9C···O7i | 0.90 | 2.22 | 2.978 (5) | 141 |
N11—H11C···O1i | 0.90 | 2.13 | 2.955 (5) | 151 |
N9—H9D···Cl1i | 0.90 | 2.52 | 3.297 (4) | 146 |
O9W—H9WD···Cl1i | 0.85 | 2.57 | 3.270 (12) | 140 |
N12—H12C···O8vi | 0.90 | 2.30 | 3.106 (5) | 148 |
N11—H11D···O3Wvii | 0.90 | 2.18 | 3.071 (14) | 169 |
N10—H10D···O3Wvii | 0.90 | 2.24 | 3.032 (12) | 147 |
N12—H12D···Cl3v | 0.90 | 2.54 | 3.341 (4) | 149 |
O7—H7E···O5viii | 0.82 | 1.91 | 2.717 (5) | 167 |
O14—H14D···O11ix | 0.82 | 1.94 | 2.679 (5) | 150 |
O1W—H1WB···Cl3ix | 0.85 | 2.28 | 3.078 (4) | 157 |
Symmetry codes: (i) −x+1, −y+1, −z+2; (iii) −x+1, −y+1, −z+1; (iv) x, y, z−1; (v) x, y+1, z; (vi) −x+2, −y+1, −z+1; (vii) x+1, y, z; (viii) −x, −y+1, −z+2; (ix) −x+1, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Co(C2H8N2)3]2[Ru2Cl2(C2H4O7P2)2]Cl·3H2O |
Mr | 1245.01 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 10.5166 (16), 15.297 (2), 15.497 (2) |
α, β, γ (°) | 90.788 (3), 91.362 (4), 96.273 (3) |
V (Å3) | 2477.2 (6) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.61 |
Crystal size (mm) | 0.3 × 0.2 × 0.2 |
Data collection | |
Diffractometer | Bruker SMART APEX CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2000) |
Tmin, Tmax | 0.69, 0.72 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12440, 8573, 6430 |
Rint | 0.047 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.109, 1.09 |
No. of reflections | 8573 |
No. of parameters | 559 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.39, −0.37 |
Computer programs: SMART (Bruker, 2000), SMART, SAINT (Bruker, 2000), SHELXTL (Bruker, 2000), SHELXTL.
D—H···A | D—H | H···A | D···A | D—H···A |
O3W—H3WD···O2W | 0.85 | 2.23 | 3.081 (18) | 174 |
O1W—H1WA···O10 | 0.85 | 1.86 | 2.663 (4) | 157 |
N7—H7D···O9W | 0.90 | 2.19 | 3.062 (13) | 162 |
N6—H6D···O5W | 0.90 | 2.19 | 2.999 (14) | 150 |
N1—H1C···O11i | 0.90 | 2.13 | 3.001 (5) | 162 |
N4—H4C···O11i | 0.90 | 2.24 | 3.079 (5) | 154 |
N5—H5C···Cl3i | 0.90 | 2.54 | 3.320 (4) | 146 |
N6—H6C···O2i | 0.90 | 1.99 | 2.872 (5) | 167 |
O2W—H2WB···O7Wi | 0.85 | 2.46 | 3.268 (19) | 159 |
O4W—H4WA···O6Wi | 0.85 | 1.97 | 2.773 (19) | 157 |
O6W—H6WC···O4Wi | 0.85 | 1.98 | 2.773 (19) | 156 |
N2—H2C···O6ii | 0.90 | 2.48 | 3.282 (5) | 148 |
N3—H3C···Cl1ii | 0.90 | 2.40 | 3.197 (4) | 148 |
N7—H7C···O12iii | 0.90 | 2.37 | 3.161 (5) | 147 |
N8—H8D···Cl3iii | 0.90 | 2.33 | 3.193 (4) | 160 |
N10—H10C···Cl2iii | 0.90 | 2.56 | 3.323 (4) | 143 |
O4W—H4WC···O9iii | 0.85 | 1.59 | 2.429 (15) | 169 |
N8—H8C···O3iv | 0.90 | 2.03 | 2.906 (5) | 164 |
N9—H9C···O7iv | 0.90 | 2.22 | 2.978 (5) | 141 |
N11—H11C···O1iv | 0.90 | 2.13 | 2.955 (5) | 151 |
N9—H9D···Cl1iv | 0.90 | 2.52 | 3.297 (4) | 146 |
O9W—H9WD···Cl1iv | 0.85 | 2.57 | 3.270 (12) | 140 |
N12—H12C···O8v | 0.90 | 2.30 | 3.106 (5) | 148 |
N11—H11D···O3Wvi | 0.90 | 2.18 | 3.071 (14) | 169 |
N10—H10D···O3Wvi | 0.90 | 2.24 | 3.032 (12) | 147 |
N12—H12D···Cl3iii | 0.90 | 2.54 | 3.341 (4) | 149 |
O7—H7E···O5vii | 0.82 | 1.91 | 2.717 (5) | 167 |
O14—H14D···O11viii | 0.82 | 1.94 | 2.679 (5) | 150 |
O1W—H1WB···Cl3viii | 0.85 | 2.28 | 3.078 (4) | 157 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y, z−1; (iii) x, y+1, z; (iv) −x+1, −y+1, −z+2; (v) −x+2, −y+1, −z+1; (vi) x+1, y, z; (vii) −x, −y+1, −z+2; (viii) −x+1, −y, −z+1. |
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Metal phosphonates are organic–inorganic hybrid materials that are important because of their potential applications in ion exchange, sensors, catalysis and molecular recognition (Clearfield et al., 1998; Cao et al., 1992; Zheng et al., 2000; Katz et al., 1991; Alberti et al., 1996). Although a number of new compounds have been reported, examples of ruthenium phosphonate compounds are extremely limited (Yi et al., 2003; Macann et al., 1993). In a previous paper, we described the synthesis of a ruthenium–hedp compound, (NH4)3Ru2(hedp)2·2H2O [hedp is 1-hydroxyethylidenediphosphonate, CH3C(OH)(PO3)2], which exhibits a novel two-dimensional structure. We present here the synthesis and structure of a new ruthenium phosphonate compound, namely [(Co(en)3)]2[Ru2(hedp)2Cl2]Cl·5H2O, (I).
Compound 1 has a three-dimensional open-network structure, composed of [Ru2(hedp)2Cl2]5− anions and [Co(en)3]3+ cations. As shown in Fig. 1, there are two crystallographically independent Ru atoms, each having a distorted octahedral environment, with the four basal positions occupied by phosphonate O atoms from two equivalent hedp ligands (O3, O6, O2A and O4A for atom Ru1,and O9, O12, O8A and O13A for atom Ru2). The Ru—O bond distances range from 2.000 (3) to 2.047 (3) Å and the O—Ru—O bond angles from 88.40 (13) to 88.42 (9)°. One axial position of each Ru octahedron is occupied by a Cl− anion and the other site is filled by the equivalent Ru atom. The Ru1—Cl1 and Ru2—Cl2 bond distances are 2.600 (8) and 2.553 (13) Å, respectively. Each hedp serves as a bis-chelating bridging ligand, linking the two equivalent Ru atoms via four phosphonate O atoms, thus forming [Ru2(hedp)2Cl2]5− dimers. The remaining two phosphonated O atoms are pendent. The Ru1—Ru1A and Ru2—Ru2A bond distances are 2.359 (8) and 2.379 (8) Å, respectively. These values are in agreement with those reported for (NH4)3Ru2(hedp)2·2H2O. Inversion centers are located at the mid-points of the Ru1—Ru1A and Ru2—Ru2A bonds.
The diruthenium units, Ru12 and Ru22, are each linked to their equivalents via O···O hydrogen bonds [O7—H7E···O5i = 2.717 (5) Å for Ru12, and O14—H14D···O11ii = 2.679 (5) Å for Ru22; symmetry codes: (i) −x,1 − y,2 − z; (ii) 1 − x,-y,1 − z], forming two types of chains along the a axis (Fig. 2). The chains are separated by [Co(en)3]3+ cations, with extensive intermolecular hydrogen bonding [N3—H3c···O2iii = 3.006 (5) Å, N6—H6C···O6iv = 3.040 (5) Å, N6—H6C···O2iii = 2.875 Å, N8—H8C···O3v = 2.905 (6) Å, N9—H9C···O7v = 2.978 (5) Å, N9—H9C···Ov = 3.052 (5) Å and N11—H11C···O1v = 2.955 (5) Å for Ru12, and N1—H1C···O11iii = 3.001 (6) Å and N10—H10···O8vi = 2.967 (5) Å for Ru22; symmetry codes: (iii) 1 − x,1 − y,1 − z; (iv) x,y,-1 + z; (v) 1 − x,1 − y,2 − z; (vi) 2 − x,1 − y,1 − z]. Consequently, a three-dimensional supramolecular open-network structure is constructed, with channels generated along the [100] direction (Fig. 3). The uncoordinated water molecules and chloride anions reside within these channels. Although each [Co(en)3]3+ ion is chiral, the overall structure of (I) is not chiral because each [Co(en)3]3+ is centrosymmetrically related to its equivalent.