Literature DB >> 21587692

Tris(2,2'-bipyridine)-cobalt(II) μ(6)-oxido-dodeca-μ(2)-oxido-hexa-oxidohexa-molydate(VI).

Ying Liu1, Xianxi Zhang, Zechun Xue, Jian Sheng.   

Abstract

In the title compound, [Co(C(10)H(8)N(2))(3)][Mo(6)O(19)], the Co(2+) cation is surrounded in a distorted octa-hedral coordination by six N atoms from three 2,2'-bipyridine ligands. The distribution of Mo-O bond lengths in the Lindqvist isopolyanion is consistent with other structures containing the same unit. In the crystal, the cations and anions are linked by C-H⋯O inter-actions.

Entities:  

Year:  2010        PMID: 21587692      PMCID: PMC3006945          DOI: 10.1107/S1600536810020775

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For general background to polyoxometalates, see: Pope & Müller (1991 ▶). For polyoxometalates modified with amines, see: Zhang, Dou et al. (2009 ▶); Zhang, Wei et al. (2009 ▶). For another structure containing the μ6-oxido-dodeca­kis­-μ2-oxido-hexaoxidohexamolydate(VI) anion see: Dahlstrom et al. (1982 ▶). For Co—N bond lengths in a related structure, see: Li & Xu (2009 ▶).

Experimental

Crystal data

[Co(C10H8N2)3][Mo6O19] M = 1407.12 Monoclinic, a = 12.310 (2) Å b = 18.979 (4) Å c = 17.150 (4) Å β = 100.895 (3)° V = 3934.4 (14) Å3 Z = 4 Mo Kα radiation μ = 2.35 mm−1 T = 296 K 0.12 × 0.10 × 0.08 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.766, T max = 0.834 25652 measured reflections 6500 independent reflections 4649 reflections with I > 2σ(I) R int = 0.041

Refinement

R[F 2 > 2σ(F 2)] = 0.032 wR(F 2) = 0.092 S = 1.00 6500 reflections 559 parameters H-atom parameters constrained Δρmax = 0.65 e Å−3 Δρmin = −0.54 e Å−3 Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810020775/hb5476sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810020775/hb5476Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Co(C10H8N2)3][Mo6O19]F(000) = 2708
Mr = 1407.12Dx = 2.376 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 2413 reflections
a = 12.310 (2) Åθ = 2.4–24.3°
b = 18.979 (4) ŵ = 2.35 mm1
c = 17.150 (4) ÅT = 296 K
β = 100.895 (3)°Block, red
V = 3934.4 (14) Å30.12 × 0.10 × 0.08 mm
Z = 4
Bruker APEXII CCD diffractometer6500 independent reflections
Radiation source: fine-focus sealed tube4649 reflections with I > 2σ(I)
graphiteRint = 0.041
φ and ω scansθmax = 24.5°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2001)h = −14→13
Tmin = 0.766, Tmax = 0.834k = −22→22
25652 measured reflectionsl = −18→19
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.092H-atom parameters constrained
S = 1.00w = 1/[σ2(Fo2) + (0.041P)2 + 10.1791P] where P = (Fo2 + 2Fc2)/3
6500 reflections(Δ/σ)max = 0.003
559 parametersΔρmax = 0.65 e Å3
0 restraintsΔρmin = −0.54 e Å3
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.
xyzUiso*/Ueq
C10.8841 (6)0.1849 (4)0.0079 (4)0.0458 (17)
H10.89620.13710.00080.055*
C20.9125 (6)0.2314 (4)−0.0452 (4)0.0523 (19)
H20.94380.2154−0.08730.063*
C30.8947 (7)0.3012 (4)−0.0362 (4)0.061 (2)
H30.91300.3336−0.07230.073*
C40.8498 (6)0.3235 (4)0.0264 (4)0.0526 (19)
H40.83780.37120.03380.063*
C50.8221 (5)0.2735 (3)0.0793 (4)0.0395 (15)
C60.7754 (5)0.2926 (3)0.1498 (4)0.0355 (14)
C70.7683 (6)0.3610 (3)0.1751 (4)0.0478 (17)
H70.78960.39820.14610.057*
C80.7294 (6)0.3736 (4)0.2435 (4)0.0554 (19)
H80.72500.41960.26150.066*
C90.6975 (5)0.3189 (4)0.2848 (4)0.0472 (17)
H90.67110.32650.33150.057*
C100.7051 (5)0.2527 (4)0.2561 (4)0.0425 (16)
H100.68300.21520.28430.051*
C110.5497 (5)0.1943 (4)0.0374 (4)0.0478 (17)
H110.54920.22820.07650.057*
C120.4747 (6)0.1997 (5)−0.0318 (5)0.063 (2)
H120.42480.2369−0.03980.076*
C130.4737 (7)0.1496 (5)−0.0891 (5)0.078 (3)
H130.42250.1521−0.13640.094*
C140.5478 (6)0.0964 (5)−0.0764 (4)0.065 (2)
H140.54840.0622−0.11510.078*
C150.6226 (5)0.0931 (4)−0.0056 (4)0.0427 (16)
C160.7059 (6)0.0373 (3)0.0130 (4)0.0447 (16)
C170.7080 (7)−0.0232 (4)−0.0324 (5)0.067 (2)
H170.6542−0.0295−0.07790.080*
C180.7867 (8)−0.0727 (4)−0.0117 (6)0.079 (3)
H180.7881−0.1130−0.04230.095*
C190.8636 (7)−0.0623 (4)0.0551 (5)0.063 (2)
H190.9189−0.09550.07090.076*
C200.8592 (6)−0.0022 (4)0.0993 (4)0.0542 (19)
H200.91240.00430.14500.065*
C211.0059 (5)0.1421 (3)0.2316 (4)0.0452 (17)
H211.02360.15870.18450.054*
C221.0883 (6)0.1384 (4)0.2973 (4)0.0529 (19)
H221.16040.15150.29490.063*
C230.9551 (5)0.0950 (4)0.3682 (4)0.0472 (17)
H230.93600.07910.41510.057*
C240.8764 (5)0.0987 (3)0.2994 (3)0.0329 (14)
C250.7600 (5)0.0778 (3)0.2945 (4)0.0330 (14)
C260.7195 (6)0.0507 (3)0.3593 (4)0.0454 (17)
H260.76570.04430.40830.054*
C270.6079 (6)0.0339 (4)0.3479 (4)0.0519 (18)
H270.57840.01590.38980.062*
C280.5422 (6)0.0433 (4)0.2765 (4)0.0511 (18)
H280.46750.03160.26860.061*
C290.5867 (5)0.0701 (4)0.2165 (4)0.0451 (17)
H290.54100.07710.16730.054*
C301.0613 (6)0.1148 (4)0.3668 (5)0.0531 (19)
H301.11510.11240.41280.064*
Co10.76522 (6)0.13938 (4)0.14146 (4)0.02958 (19)
Mo10.62552 (4)0.16746 (3)0.70535 (3)0.03880 (16)
Mo20.68058 (5)0.03933 (3)0.59227 (3)0.03863 (15)
Mo30.93267 (4)0.09804 (3)0.60537 (3)0.04001 (16)
Mo40.72000 (5)0.20190 (3)0.54351 (3)0.04164 (16)
Mo50.87672 (5)0.22739 (3)0.71735 (4)0.04679 (17)
Mo60.83628 (5)0.06397 (3)0.76648 (3)0.04393 (17)
N10.8397 (4)0.2045 (3)0.0694 (3)0.0371 (12)
N20.7428 (4)0.2385 (3)0.1891 (3)0.0355 (12)
N30.6238 (4)0.1425 (3)0.0512 (3)0.0421 (13)
N40.7816 (4)0.0472 (3)0.0790 (3)0.0401 (13)
N50.6935 (4)0.0870 (3)0.2251 (3)0.0395 (13)
N60.9018 (4)0.1232 (3)0.2313 (3)0.0373 (12)
O10.6778 (4)0.2537 (3)0.4646 (3)0.0632 (14)
O20.8518 (4)0.1606 (2)0.5229 (3)0.0467 (11)
O30.6467 (3)0.1147 (2)0.5161 (2)0.0424 (11)
O40.9808 (3)0.1811 (2)0.6620 (3)0.0492 (12)
O50.8119 (4)0.2659 (2)0.6171 (3)0.0518 (12)
O60.9511 (4)0.2935 (3)0.7643 (3)0.0744 (17)
O70.6093 (3)0.2189 (2)0.6099 (3)0.0447 (11)
O80.7392 (4)0.2354 (2)0.7496 (3)0.0494 (12)
O90.5168 (4)0.1929 (3)0.7438 (3)0.0539 (12)
O100.7046 (3)0.1044 (2)0.7871 (3)0.0484 (12)
O110.9111 (4)0.1509 (3)0.7929 (3)0.0518 (12)
O120.7786 (3)0.13302 (19)0.6550 (2)0.0329 (9)
O130.5755 (3)0.0853 (2)0.6474 (3)0.0419 (11)
O140.8815 (4)0.0131 (3)0.8463 (3)0.0705 (16)
O150.7458 (4)0.0007 (2)0.6930 (3)0.0485 (12)
O160.9500 (3)0.0484 (2)0.7010 (3)0.0475 (12)
O170.6077 (4)−0.0283 (2)0.5469 (3)0.0600 (14)
O180.8188 (3)0.0303 (2)0.5606 (2)0.0438 (11)
O191.0407 (4)0.0735 (3)0.5655 (3)0.0565 (13)
U11U22U33U12U13U23
C10.057 (4)0.042 (4)0.041 (4)−0.006 (3)0.017 (3)−0.004 (3)
C20.064 (5)0.061 (5)0.034 (4)−0.010 (4)0.015 (4)−0.004 (4)
C30.086 (6)0.055 (5)0.043 (4)−0.018 (4)0.015 (4)0.010 (4)
C40.079 (5)0.036 (4)0.041 (4)−0.006 (4)0.006 (4)0.006 (3)
C50.036 (4)0.048 (4)0.032 (4)−0.004 (3)0.001 (3)0.002 (3)
C60.036 (4)0.033 (4)0.034 (4)−0.003 (3)−0.002 (3)−0.001 (3)
C70.061 (5)0.030 (4)0.050 (4)−0.001 (3)0.006 (4)−0.002 (3)
C80.064 (5)0.042 (4)0.057 (5)0.009 (4)0.003 (4)−0.016 (4)
C90.049 (4)0.049 (4)0.043 (4)0.009 (3)0.008 (3)−0.011 (4)
C100.043 (4)0.055 (4)0.029 (4)0.011 (3)0.005 (3)0.005 (3)
C110.048 (4)0.055 (4)0.040 (4)0.011 (4)0.009 (3)−0.003 (3)
C120.043 (4)0.089 (6)0.056 (5)0.028 (4)0.007 (4)0.004 (5)
C130.045 (5)0.128 (8)0.056 (5)0.025 (5)−0.001 (4)−0.008 (6)
C140.053 (5)0.091 (6)0.048 (5)0.005 (5)0.002 (4)−0.022 (4)
C150.036 (4)0.054 (4)0.038 (4)−0.008 (3)0.006 (3)−0.006 (3)
C160.055 (4)0.035 (4)0.048 (4)−0.009 (3)0.017 (4)−0.003 (3)
C170.083 (6)0.051 (5)0.060 (5)−0.005 (4)0.000 (4)−0.018 (4)
C180.115 (8)0.039 (5)0.087 (7)0.003 (5)0.029 (6)−0.021 (5)
C190.076 (6)0.040 (4)0.080 (6)0.011 (4)0.030 (5)0.004 (4)
C200.055 (5)0.050 (5)0.057 (5)0.012 (4)0.011 (4)0.006 (4)
C210.046 (4)0.041 (4)0.050 (4)−0.004 (3)0.013 (3)0.005 (3)
C220.038 (4)0.048 (4)0.068 (5)−0.006 (3)0.000 (4)0.006 (4)
C230.047 (4)0.051 (4)0.040 (4)0.007 (3)0.000 (3)0.004 (3)
C240.045 (4)0.025 (3)0.029 (3)0.005 (3)0.008 (3)−0.001 (3)
C250.039 (4)0.026 (3)0.034 (4)−0.001 (3)0.008 (3)−0.005 (3)
C260.056 (5)0.045 (4)0.036 (4)−0.001 (3)0.011 (3)0.003 (3)
C270.058 (5)0.054 (4)0.049 (4)−0.008 (4)0.022 (4)0.004 (4)
C280.043 (4)0.057 (5)0.055 (5)−0.011 (3)0.013 (4)0.003 (4)
C290.039 (4)0.057 (4)0.037 (4)−0.010 (3)0.003 (3)0.004 (3)
C300.042 (4)0.046 (4)0.065 (5)0.002 (3)−0.006 (4)0.005 (4)
Co10.0301 (4)0.0305 (4)0.0280 (4)−0.0009 (3)0.0050 (3)0.0012 (3)
Mo10.0331 (3)0.0401 (3)0.0451 (3)0.0020 (2)0.0123 (3)−0.0020 (3)
Mo20.0368 (3)0.0331 (3)0.0451 (4)−0.0059 (2)0.0056 (3)−0.0064 (3)
Mo30.0320 (3)0.0490 (4)0.0402 (3)0.0000 (3)0.0099 (3)−0.0069 (3)
Mo40.0430 (3)0.0396 (3)0.0428 (3)0.0011 (3)0.0094 (3)0.0095 (3)
Mo50.0413 (3)0.0481 (4)0.0522 (4)−0.0139 (3)0.0117 (3)−0.0186 (3)
Mo60.0384 (3)0.0556 (4)0.0369 (3)0.0076 (3)0.0049 (3)0.0077 (3)
N10.042 (3)0.039 (3)0.030 (3)−0.003 (2)0.007 (2)−0.002 (2)
N20.036 (3)0.041 (3)0.028 (3)0.001 (2)0.001 (2)0.001 (2)
N30.037 (3)0.045 (3)0.045 (3)0.001 (3)0.008 (3)0.003 (3)
N40.040 (3)0.038 (3)0.042 (3)−0.001 (2)0.007 (3)0.000 (3)
N50.042 (3)0.037 (3)0.039 (3)−0.004 (2)0.006 (3)0.004 (2)
N60.035 (3)0.036 (3)0.040 (3)−0.005 (2)0.005 (2)0.003 (2)
O10.063 (3)0.067 (3)0.060 (3)0.004 (3)0.014 (3)0.027 (3)
O20.046 (3)0.053 (3)0.044 (3)−0.002 (2)0.015 (2)0.002 (2)
O30.035 (2)0.049 (3)0.039 (3)−0.003 (2)−0.004 (2)0.001 (2)
O40.036 (3)0.062 (3)0.049 (3)−0.012 (2)0.007 (2)−0.014 (2)
O50.054 (3)0.032 (2)0.073 (3)−0.008 (2)0.019 (3)0.003 (2)
O60.063 (3)0.069 (4)0.090 (4)−0.023 (3)0.012 (3)−0.036 (3)
O70.041 (3)0.040 (3)0.054 (3)0.005 (2)0.011 (2)0.004 (2)
O80.044 (3)0.051 (3)0.056 (3)−0.001 (2)0.015 (2)−0.021 (2)
O90.039 (3)0.066 (3)0.061 (3)0.006 (2)0.018 (2)0.000 (3)
O100.043 (3)0.064 (3)0.042 (3)0.007 (2)0.016 (2)0.009 (2)
O110.040 (3)0.070 (3)0.043 (3)−0.004 (2)0.003 (2)−0.012 (2)
O120.032 (2)0.031 (2)0.038 (2)−0.0016 (18)0.0104 (18)−0.0038 (19)
O130.034 (2)0.038 (2)0.054 (3)−0.0053 (19)0.008 (2)0.001 (2)
O140.056 (3)0.096 (4)0.057 (3)0.017 (3)0.006 (3)0.026 (3)
O150.050 (3)0.036 (2)0.059 (3)−0.001 (2)0.008 (2)0.010 (2)
O160.039 (3)0.059 (3)0.043 (3)0.007 (2)0.005 (2)−0.001 (2)
O170.057 (3)0.043 (3)0.079 (4)−0.010 (2)0.008 (3)−0.018 (3)
O180.044 (3)0.044 (3)0.043 (3)0.004 (2)0.008 (2)−0.010 (2)
O190.041 (3)0.080 (4)0.050 (3)0.006 (2)0.014 (2)−0.009 (3)
C1—N11.330 (8)C25—C261.398 (8)
C1—C21.361 (9)C26—C271.387 (9)
C1—H10.9300C26—H260.9300
C2—C31.358 (10)C27—C281.346 (9)
C2—H20.9300C27—H270.9300
C3—C41.364 (10)C28—C291.354 (9)
C3—H30.9300C28—H280.9300
C4—C51.400 (9)C29—N51.334 (8)
C4—H40.9300C29—H290.9300
C5—N11.343 (8)C30—H300.9300
C5—C61.479 (8)Co1—N52.075 (5)
C6—N21.331 (7)Co1—N62.078 (5)
C6—C71.376 (8)Co1—N12.079 (5)
C7—C81.367 (9)Co1—N42.081 (5)
C7—H70.9300Co1—N22.091 (5)
C8—C91.358 (10)Co1—N32.100 (5)
C8—H80.9300Mo1—O91.671 (4)
C9—C101.359 (9)Mo1—O71.884 (4)
C9—H90.9300Mo1—O131.888 (4)
C10—N21.345 (7)Mo1—O81.948 (4)
C10—H100.9300Mo1—O101.957 (4)
C11—N31.331 (8)Mo1—O122.310 (4)
C11—C121.362 (9)Mo2—O171.671 (4)
C11—H110.9300Mo2—O181.888 (4)
C12—C131.366 (11)Mo2—O151.909 (4)
C12—H120.9300Mo2—O31.929 (4)
C13—C141.350 (11)Mo2—O131.948 (4)
C13—H130.9300Mo2—O122.299 (4)
C14—C151.379 (9)Mo3—O191.673 (4)
C14—H140.9300Mo3—O161.868 (4)
C15—N31.350 (8)Mo3—O41.888 (4)
C15—C161.467 (9)Mo3—O181.950 (4)
C16—N41.336 (8)Mo3—O21.968 (4)
C16—C171.390 (9)Mo3—O122.318 (4)
C17—C181.349 (11)Mo4—O11.673 (5)
C17—H170.9300Mo4—O21.894 (4)
C18—C191.354 (11)Mo4—O31.900 (4)
C18—H180.9300Mo4—O51.951 (5)
C19—C201.377 (10)Mo4—O71.961 (4)
C19—H190.9300Mo4—O122.316 (4)
C20—N41.336 (8)Mo5—O61.669 (5)
C20—H200.9300Mo5—O81.884 (4)
C21—N61.330 (8)Mo5—O51.900 (5)
C21—C221.368 (9)Mo5—O111.939 (5)
C21—H210.9300Mo5—O41.943 (4)
C22—C301.373 (10)Mo5—O122.307 (4)
C22—H220.9300Mo6—O141.682 (5)
C23—C301.365 (9)Mo6—O101.887 (4)
C23—C241.379 (8)Mo6—O111.902 (5)
C23—H230.9300Mo6—O151.934 (4)
C24—N61.347 (7)Mo6—O161.976 (4)
C24—C251.474 (8)Mo6—O122.316 (4)
C25—N51.323 (7)
N1—C1—C2123.1 (7)O17—Mo2—O18103.3 (2)
N1—C1—H1118.5O17—Mo2—O15102.9 (2)
C2—C1—H1118.5O18—Mo2—O1588.73 (19)
C3—C2—C1119.3 (7)O17—Mo2—O3103.1 (2)
C3—C2—H2120.3O18—Mo2—O387.96 (18)
C1—C2—H2120.3O15—Mo2—O3153.89 (18)
C2—C3—C4119.4 (7)O17—Mo2—O13102.9 (2)
C2—C3—H3120.3O18—Mo2—O13153.82 (17)
C4—C3—H3120.3O15—Mo2—O1386.36 (19)
C3—C4—C5119.0 (7)O3—Mo2—O1385.28 (18)
C3—C4—H4120.5O17—Mo2—O12179.2 (2)
C5—C4—H4120.5O18—Mo2—O1277.50 (15)
N1—C5—C4120.9 (6)O15—Mo2—O1277.28 (16)
N1—C5—C6116.1 (5)O3—Mo2—O1276.72 (16)
C4—C5—C6123.0 (6)O13—Mo2—O1276.34 (15)
N2—C6—C7121.6 (6)O19—Mo3—O16104.5 (2)
N2—C6—C5115.2 (5)O19—Mo3—O4104.3 (2)
C7—C6—C5123.2 (6)O16—Mo3—O489.9 (2)
C8—C7—C6119.3 (7)O19—Mo3—O18102.9 (2)
C8—C7—H7120.4O16—Mo3—O1888.10 (19)
C6—C7—H7120.4O4—Mo3—O18152.37 (18)
C9—C8—C7119.8 (6)O19—Mo3—O2102.0 (2)
C9—C8—H8120.1O16—Mo3—O2153.38 (18)
C7—C8—H8120.1O4—Mo3—O286.13 (19)
C8—C9—C10118.1 (6)O18—Mo3—O283.50 (18)
C8—C9—H9120.9O19—Mo3—O12177.44 (19)
C10—C9—H9120.9O16—Mo3—O1277.75 (16)
N2—C10—C9123.6 (6)O4—Mo3—O1276.77 (16)
N2—C10—H10118.2O18—Mo3—O1275.87 (15)
C9—C10—H10118.2O2—Mo3—O1275.71 (16)
N3—C11—C12122.6 (7)O1—Mo4—O2103.8 (2)
N3—C11—H11118.7O1—Mo4—O3104.5 (2)
C12—C11—H11118.7O2—Mo4—O388.71 (19)
C13—C12—C11119.1 (7)O1—Mo4—O5102.2 (2)
C13—C12—H12120.5O2—Mo4—O588.06 (19)
C11—C12—H12120.5O3—Mo4—O5153.15 (18)
C14—C13—C12119.4 (7)O1—Mo4—O7103.3 (2)
C14—C13—H13120.3O2—Mo4—O7152.92 (18)
C12—C13—H13120.3O3—Mo4—O786.39 (18)
C13—C14—C15119.6 (7)O5—Mo4—O784.46 (19)
C13—C14—H14120.2O1—Mo4—O12178.4 (2)
C15—C14—H14120.2O2—Mo4—O1277.12 (16)
N3—C15—C14121.2 (7)O3—Mo4—O1276.83 (15)
N3—C15—C16115.6 (6)O5—Mo4—O1276.46 (16)
C14—C15—C16123.2 (6)O7—Mo4—O1275.83 (15)
N4—C16—C17120.5 (7)O6—Mo5—O8103.8 (2)
N4—C16—C15115.5 (6)O6—Mo5—O5104.2 (2)
C17—C16—C15124.0 (7)O8—Mo5—O589.3 (2)
C18—C17—C16121.0 (8)O6—Mo5—O11102.1 (3)
C18—C17—H17119.5O8—Mo5—O1187.6 (2)
C16—C17—H17119.5O5—Mo5—O11153.44 (19)
C17—C18—C19118.2 (8)O6—Mo5—O4102.9 (2)
C17—C18—H18120.9O8—Mo5—O4153.17 (18)
C19—C18—H18120.9O5—Mo5—O486.3 (2)
C18—C19—C20119.6 (8)O11—Mo5—O484.69 (19)
C18—C19—H19120.2O6—Mo5—O12177.9 (2)
C20—C19—H19120.2O8—Mo5—O1277.15 (16)
N4—C20—C19122.6 (7)O5—Mo5—O1277.63 (16)
N4—C20—H20118.7O11—Mo5—O1275.97 (16)
C19—C20—H20118.7O4—Mo5—O1276.05 (15)
N6—C21—C22123.6 (6)O14—Mo6—O10104.1 (2)
N6—C21—H21118.2O14—Mo6—O11103.5 (2)
C22—C21—H21118.2O10—Mo6—O1189.9 (2)
C21—C22—C30117.9 (7)O14—Mo6—O15103.6 (2)
C21—C22—H22121.0O10—Mo6—O1588.0 (2)
C30—C22—H22121.0O11—Mo6—O15152.55 (19)
C30—C23—C24119.4 (7)O14—Mo6—O16102.5 (2)
C30—C23—H23120.3O10—Mo6—O16153.36 (18)
C24—C23—H23120.3O11—Mo6—O1684.39 (19)
N6—C24—C23121.2 (6)O15—Mo6—O1685.39 (19)
N6—C24—C25115.2 (5)O14—Mo6—O12178.3 (2)
C23—C24—C25123.6 (6)O10—Mo6—O1277.53 (16)
N5—C25—C26120.7 (6)O11—Mo6—O1276.43 (17)
N5—C25—C24116.5 (5)O15—Mo6—O1276.39 (15)
C26—C25—C24122.9 (6)O16—Mo6—O1275.83 (16)
C27—C26—C25117.7 (6)C1—N1—C5118.3 (5)
C27—C26—H26121.2C1—N1—Co1126.7 (4)
C25—C26—H26121.2C5—N1—Co1113.9 (4)
C28—C27—C26120.5 (6)C6—N2—C10117.6 (6)
C28—C27—H27119.8C6—N2—Co1114.9 (4)
C26—C27—H27119.8C10—N2—Co1127.3 (4)
C27—C28—C29118.8 (7)C11—N3—C15118.0 (6)
C27—C28—H28120.6C11—N3—Co1126.6 (5)
C29—C28—H28120.6C15—N3—Co1114.0 (4)
N5—C29—C28122.6 (6)C20—N4—C16118.1 (6)
N5—C29—H29118.7C20—N4—Co1126.1 (5)
C28—C29—H29118.7C16—N4—Co1115.7 (4)
C23—C30—C22119.7 (7)C25—N5—C29119.8 (5)
C23—C30—H30120.2C25—N5—Co1114.4 (4)
C22—C30—H30120.2C29—N5—Co1125.3 (4)
N5—Co1—N678.9 (2)C21—N6—C24118.1 (6)
N5—Co1—N1171.4 (2)C21—N6—Co1127.3 (4)
N6—Co1—N198.20 (19)C24—N6—Co1114.0 (4)
N5—Co1—N492.8 (2)Mo4—O2—Mo3116.7 (2)
N6—Co1—N496.5 (2)Mo4—O3—Mo2116.5 (2)
N1—Co1—N495.6 (2)Mo3—O4—Mo5117.2 (2)
N5—Co1—N293.2 (2)Mo5—O5—Mo4116.0 (2)
N6—Co1—N289.51 (19)Mo1—O7—Mo4116.6 (2)
N1—Co1—N278.62 (19)Mo5—O8—Mo1116.8 (2)
N4—Co1—N2172.2 (2)Mo6—O10—Mo1116.3 (2)
N5—Co1—N397.0 (2)Mo6—O11—Mo5117.1 (2)
N6—Co1—N3173.0 (2)Mo2—O12—Mo5179.7 (2)
N1—Co1—N386.7 (2)Mo2—O12—Mo190.06 (13)
N4—Co1—N378.0 (2)Mo5—O12—Mo189.99 (13)
N2—Co1—N396.3 (2)Mo2—O12—Mo489.78 (14)
O9—Mo1—O7103.4 (2)Mo5—O12—Mo489.91 (13)
O9—Mo1—O13103.9 (2)Mo1—O12—Mo490.02 (13)
O7—Mo1—O1390.01 (18)Mo2—O12—Mo690.04 (13)
O9—Mo1—O8103.0 (2)Mo5—O12—Mo690.27 (14)
O7—Mo1—O886.9 (2)Mo1—O12—Mo689.78 (13)
O13—Mo1—O8152.92 (17)Mo4—O12—Mo6179.7 (2)
O9—Mo1—O10102.8 (2)Mo2—O12—Mo390.00 (13)
O7—Mo1—O10153.66 (18)Mo5—O12—Mo389.96 (13)
O13—Mo1—O1086.59 (19)Mo1—O12—Mo3179.6 (2)
O8—Mo1—O1084.4 (2)Mo4—O12—Mo390.40 (13)
O9—Mo1—O12178.6 (2)Mo6—O12—Mo389.79 (13)
O7—Mo1—O1277.40 (16)Mo1—O13—Mo2116.4 (2)
O13—Mo1—O1277.16 (15)Mo2—O15—Mo6116.3 (2)
O8—Mo1—O1275.91 (15)Mo3—O16—Mo6116.6 (2)
O10—Mo1—O1276.38 (15)Mo2—O18—Mo3116.5 (2)
D—H···AD—HH···AD···AD—H···A
C2—H2···O11i0.932.363.166 (9)145
C4—H4···O17ii0.932.523.165 (9)127
C11—H11···O4iii0.932.513.400 (8)161
C12—H12···O2iii0.932.473.277 (10)145
C20—H20···O14iv0.932.533.159 (9)125
C22—H22···O8v0.932.543.230 (9)132
C26—H26···O180.932.583.459 (8)157
Table 1

Selected bond lengths (Å)

Co1—N52.075 (5)
Co1—N62.078 (5)
Co1—N12.079 (5)
Co1—N42.081 (5)
Co1—N22.091 (5)
Co1—N32.100 (5)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
C2—H2⋯O11i0.932.363.166 (9)145
C4—H4⋯O17ii0.932.523.165 (9)127
C11—H11⋯O4iii0.932.513.400 (8)161
C12—H12⋯O2iii0.932.473.277 (10)145
C20—H20⋯O14iv0.932.533.159 (9)125
C22—H22⋯O8v0.932.543.230 (9)132
C26—H26⋯O180.932.583.459 (8)157

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

  2 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  catena-Poly[[(2,2'-bipyridine-κN,N')cobalt(II)]-μ-oxalato-κO,O:O,O].

Authors:  Pei-Zhou Li; Qiang Xu
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-04-10
  2 in total
  2 in total

1.  Tris(4,4'-di-tert-butyl-2,2'-bipyridine-κN,N')molybdenum(II) μ(6)-oxido-dodeca-μ(2)-oxido-hexa-oxidohexa-molybdate(VI) acetonitrile tetra-solvate.

Authors:  Tatiana R Amarante; José A Fernandes; Isabel S Gonçalves; Filipe A Almeida Paz
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-11-25

2.  Tris(2,2'-bipyridine-κ(2) N,N')cobalt(II) bis-(hexa-fluoridophosphate).

Authors:  Ayfer Menteş; Kuldip Singh
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-12-15
  2 in total

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