Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807046107/hb2544sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807046107/hb2544Isup2.hkl |
CCDC reference: 1296707
A mixture of cobalt dichloride (0.5 mmol), benzene-1,3-dicarboxylic acid (0.5 mmol), sodium hydroxide (1 mmol), 4,4'-bipyridine (0.5 mmol), H2O (8 ml) and ethanol (8 ml) in a 25-ml Teflon-lined stainless steel autoclave was heated at 453 K for one week, and then cooled to room temperature. Red blocks of (I) were obtained with a yield of 8%. Anal. Calc. for C27H35CoN5O12: C 47.61, H 5.14, N 10.29%; Found: C 47.56, H 5.18, N 10.22%.
The H atoms of the water molecule were located from difference density maps and were refined with distance restraints of H···H = 1.38 (2) Å and O—H = 0.82 (2) Å. All other H atoms were placed in calculated positions (C—H = 0.93 Å) and refined as riding with Uiso(H) = 1.2Ueq of the respective carrier atom.
As part of our studies of coordination polymer networks (Howell et al., 2001), the molecular title compound, (I), arose.
The Coii atom is (I) is coordinated by two monodentate 4,4'-bipyridine molecules in the axial sites and four associated water molecules in the equatorial plane with the r.m.s. deviation for the fitted atoms (Co1, O1, O2, O3, O4) being 0.012 Å (Fig. 1, Table 1). The dihedral angle between the N1 and N2 rings is 6.2 (3)°; that between the N3 and N4 rings is 6.9 (3)°.
A network of O—H···O and O—H···N hydrogen bonds (Table 2, Fig. 2) helps to establish the packing for (I).
For general background, see: Howell et al. (2001).
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL (Bruker, 2001).
[Co(C10H8N2)2(H2O)4](C7H3NO4)·4H2O | F(000) = 1420 |
Mr = 680.53 | Dx = 1.462 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C -2yc | Cell parameters from 3167 reflections |
a = 18.1827 (5) Å | θ = 1.6–25.0° |
b = 6.8537 (10) Å | µ = 0.63 mm−1 |
c = 25.1485 (5) Å | T = 293 K |
β = 99.398 (10)° | Block, red |
V = 3091.9 (5) Å3 | 0.42 × 0.28 × 0.22 mm |
Z = 4 |
Bruker APEXII CCD area-detector diffractometer | 3167 independent reflections |
Radiation source: fine-focus sealed tube | 2936 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
φ and ω scans | θmax = 25.0°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −19→21 |
Tmin = 0.779, Tmax = 0.875 | k = −8→4 |
5091 measured reflections | l = −29→12 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.043 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.129 | w = 1/[σ2(Fo2) + (0.104P)2 + 1.0603P] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max < 0.001 |
3167 reflections | Δρmax = 0.40 e Å−3 |
456 parameters | Δρmin = −0.58 e Å−3 |
26 restraints | Absolute structure: Flack (1983), with how many Friedel pairs? |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.65 (4) |
[Co(C10H8N2)2(H2O)4](C7H3NO4)·4H2O | V = 3091.9 (5) Å3 |
Mr = 680.53 | Z = 4 |
Monoclinic, Cc | Mo Kα radiation |
a = 18.1827 (5) Å | µ = 0.63 mm−1 |
b = 6.8537 (10) Å | T = 293 K |
c = 25.1485 (5) Å | 0.42 × 0.28 × 0.22 mm |
β = 99.398 (10)° |
Bruker APEXII CCD area-detector diffractometer | 3167 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 2936 reflections with I > 2σ(I) |
Tmin = 0.779, Tmax = 0.875 | Rint = 0.033 |
5091 measured reflections |
R[F2 > 2σ(F2)] = 0.043 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.129 | Δρmax = 0.40 e Å−3 |
S = 1.00 | Δρmin = −0.58 e Å−3 |
3167 reflections | Absolute structure: Flack (1983), with how many Friedel pairs? |
456 parameters | Absolute structure parameter: 0.65 (4) |
26 restraints |
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 | ||
Co1 | 0.67783 (8) | 0.76266 (9) | 0.87717 (6) | 0.0355 (2) | |
C1 | 0.6043 (3) | 0.8586 (8) | 0.9833 (2) | 0.0364 (12) | |
H1 | 0.5597 | 0.8604 | 0.9591 | 0.044* | |
C2 | 0.7306 (3) | 0.8503 (9) | 0.9992 (2) | 0.0437 (14) | |
H2 | 0.7757 | 0.8458 | 0.9864 | 0.052* | |
C3 | 0.7327 (3) | 0.8594 (8) | 1.0542 (2) | 0.0395 (13) | |
H3 | 0.7782 | 0.8620 | 1.0773 | 0.047* | |
C4 | 0.6013 (3) | 0.8673 (9) | 1.0380 (2) | 0.0389 (13) | |
H4 | 0.5556 | 0.8749 | 1.0499 | 0.047* | |
C5 | 0.6670 (3) | 0.8644 (6) | 1.0746 (2) | 0.0265 (10) | |
C6 | 0.6670 (3) | 0.8625 (7) | 1.1340 (2) | 0.0277 (11) | |
C7 | 0.6017 (3) | 0.8496 (9) | 1.1560 (2) | 0.0444 (14) | |
H7 | 0.5557 | 0.8446 | 1.1335 | 0.053* | |
C8 | 0.7334 (3) | 0.8700 (10) | 1.1714 (2) | 0.0467 (14) | |
H8 | 0.7790 | 0.8794 | 1.1594 | 0.056* | |
C9 | 0.7313 (4) | 0.8637 (9) | 1.2261 (2) | 0.0461 (14) | |
H9 | 0.7763 | 0.8682 | 1.2498 | 0.055* | |
C10 | 0.6052 (4) | 0.8443 (10) | 1.2112 (3) | 0.0553 (17) | |
H10 | 0.5605 | 0.8351 | 1.2245 | 0.066* | |
C11 | 0.6226 (3) | 0.6744 (10) | 0.7540 (2) | 0.0452 (14) | |
H11 | 0.5770 | 0.6870 | 0.7658 | 0.054* | |
C12 | 0.7481 (4) | 0.6476 (10) | 0.7726 (2) | 0.0481 (15) | |
H12 | 0.7920 | 0.6429 | 0.7974 | 0.058* | |
C13 | 0.7532 (3) | 0.6281 (10) | 0.7186 (2) | 0.0459 (14) | |
H13 | 0.7994 | 0.6063 | 0.7083 | 0.055* | |
C14 | 0.6228 (3) | 0.6587 (9) | 0.6993 (2) | 0.0430 (14) | |
H14 | 0.5777 | 0.6599 | 0.6757 | 0.052* | |
C15 | 0.6886 (3) | 0.6411 (6) | 0.6791 (2) | 0.0261 (10) | |
C16 | 0.6920 (3) | 0.6373 (6) | 0.62062 (19) | 0.0272 (11) | |
C17 | 0.6269 (3) | 0.6348 (8) | 0.5828 (2) | 0.0359 (12) | |
H17 | 0.5804 | 0.6339 | 0.5937 | 0.043* | |
C18 | 0.7592 (3) | 0.6372 (8) | 0.6013 (2) | 0.0388 (12) | |
H18 | 0.8043 | 0.6375 | 0.6249 | 0.047* | |
C19 | 0.7576 (4) | 0.6368 (8) | 0.5461 (2) | 0.0429 (13) | |
H19 | 0.8031 | 0.6383 | 0.5337 | 0.051* | |
C20 | 0.6327 (3) | 0.6335 (8) | 0.5279 (2) | 0.0379 (12) | |
H20 | 0.5889 | 0.6318 | 0.5029 | 0.045* | |
C21 | 0.4269 (3) | 0.8255 (8) | 0.6808 (2) | 0.0369 (12) | |
C22 | 0.4210 (3) | 0.9008 (7) | 0.4797 (2) | 0.0329 (10) | |
C23 | 0.4286 (6) | 0.7341 (6) | 0.6267 (4) | 0.0317 (8) | |
C24 | 0.4309 (3) | 0.5329 (7) | 0.6202 (2) | 0.0372 (11) | |
H24 | 0.4319 | 0.4520 | 0.6500 | 0.045* | |
C25 | 0.4317 (3) | 0.4511 (7) | 0.5695 (2) | 0.0381 (11) | |
H25 | 0.4338 | 0.3163 | 0.5658 | 0.046* | |
C26 | 0.4295 (3) | 0.5684 (7) | 0.5248 (2) | 0.0371 (11) | |
H26 | 0.4301 | 0.5125 | 0.4911 | 0.044* | |
C27 | 0.4265 (4) | 0.7722 (7) | 0.5299 (3) | 0.0321 (14) | |
N1 | 0.6684 (2) | 0.8477 (6) | 0.96340 (16) | 0.0301 (10) | |
N2 | 0.6678 (3) | 0.8514 (6) | 1.24685 (19) | 0.0403 (11) | |
N3 | 0.6852 (2) | 0.6725 (6) | 0.79132 (17) | 0.0325 (10) | |
N4 | 0.6963 (3) | 0.6345 (6) | 0.50961 (18) | 0.0367 (11) | |
N5 | 0.4265 (3) | 0.8515 (7) | 0.5801 (2) | 0.0432 (11) | |
O1 | 0.7932 (2) | 0.8702 (5) | 0.88665 (16) | 0.0386 (9) | |
O2 | 0.6401 (3) | 1.0475 (5) | 0.84774 (15) | 0.0448 (10) | |
O3 | 0.5623 (2) | 0.6581 (6) | 0.86976 (17) | 0.0434 (9) | |
O4 | 0.7151 (2) | 0.4793 (6) | 0.90703 (17) | 0.0445 (9) | |
O5 | 0.8406 (4) | 0.2547 (5) | 0.8925 (2) | 0.0455 (14) | |
O6 | 0.4356 (3) | 0.3084 (8) | 0.7615 (2) | 0.0700 (13) | |
O7 | 0.4362 (3) | 0.8505 (6) | 0.81861 (18) | 0.0525 (11) | |
O8 | 0.5140 (4) | 0.7287 (7) | 0.3640 (3) | 0.0559 (16) | |
O9 | 0.4161 (2) | 1.0788 (5) | 0.48651 (15) | 0.0432 (9) | |
O10 | 0.4189 (2) | 0.8175 (6) | 0.43492 (16) | 0.0446 (9) | |
O11 | 0.4273 (3) | 0.7097 (7) | 0.72046 (19) | 0.0511 (13) | |
O12 | 0.4261 (2) | 1.0060 (6) | 0.68432 (16) | 0.0459 (9) | |
H1W | 0.825 (3) | 0.793 (7) | 0.901 (3) | 0.069* | |
H2W | 0.804 (4) | 0.986 (3) | 0.892 (3) | 0.069* | |
H3W | 0.607 (3) | 1.117 (9) | 0.854 (2) | 0.069* | |
H4W | 0.645 (4) | 1.026 (10) | 0.8169 (10) | 0.069* | |
H5W | 0.526 (3) | 0.715 (8) | 0.853 (3) | 0.069* | |
H6W | 0.559 (4) | 0.5395 (18) | 0.870 (3) | 0.069* | |
H7W | 0.745 (3) | 0.416 (8) | 0.893 (3) | 0.069* | |
H8W | 0.702 (4) | 0.419 (8) | 0.932 (2) | 0.069* | |
H9W | 0.859 (4) | 0.280 (10) | 0.9234 (10) | 0.069* | |
H10W | 0.867 (4) | 0.278 (11) | 0.870 (2) | 0.069* | |
H11W | 0.415 (4) | 0.262 (8) | 0.7327 (16) | 0.069* | |
H13W | 0.458 (4) | 0.956 (5) | 0.823 (2) | 0.069* | |
H14W | 0.431 (5) | 0.813 (9) | 0.7873 (10) | 0.069* | |
H15W | 0.492 (4) | 0.739 (10) | 0.3897 (19) | 0.069* | |
H16W | 0.487 (3) | 0.724 (11) | 0.3347 (14) | 0.069* | |
H12W | 0.425 (4) | 0.422 (4) | 0.767 (3) | 0.069* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0370 (3) | 0.0440 (3) | 0.0255 (3) | 0.0009 (3) | 0.0054 (2) | 0.0012 (3) |
C1 | 0.028 (3) | 0.057 (3) | 0.023 (3) | 0.008 (2) | 0.001 (2) | −0.005 (2) |
C2 | 0.032 (3) | 0.070 (4) | 0.030 (3) | −0.007 (3) | 0.007 (2) | −0.007 (3) |
C3 | 0.027 (3) | 0.068 (3) | 0.022 (3) | −0.007 (3) | 0.001 (2) | −0.006 (2) |
C4 | 0.030 (3) | 0.066 (3) | 0.020 (3) | 0.003 (3) | 0.003 (2) | −0.003 (2) |
C5 | 0.034 (3) | 0.027 (2) | 0.019 (2) | 0.0008 (19) | 0.004 (2) | −0.0007 (18) |
C6 | 0.031 (3) | 0.029 (2) | 0.025 (3) | 0.002 (2) | 0.009 (2) | −0.0010 (18) |
C7 | 0.031 (3) | 0.071 (4) | 0.031 (3) | −0.005 (3) | 0.006 (2) | −0.005 (3) |
C8 | 0.034 (3) | 0.073 (4) | 0.034 (3) | 0.002 (3) | 0.008 (3) | 0.000 (3) |
C9 | 0.044 (3) | 0.070 (3) | 0.025 (3) | 0.003 (3) | 0.006 (3) | 0.002 (3) |
C10 | 0.054 (4) | 0.083 (4) | 0.034 (3) | −0.008 (3) | 0.021 (3) | −0.007 (3) |
C11 | 0.028 (3) | 0.084 (4) | 0.025 (3) | −0.005 (3) | 0.010 (2) | −0.007 (3) |
C12 | 0.038 (3) | 0.076 (4) | 0.028 (3) | 0.014 (3) | 0.000 (3) | −0.004 (3) |
C13 | 0.029 (3) | 0.079 (4) | 0.032 (3) | 0.008 (3) | 0.010 (2) | −0.010 (3) |
C14 | 0.023 (3) | 0.077 (4) | 0.027 (3) | −0.001 (3) | −0.002 (2) | −0.006 (3) |
C15 | 0.028 (3) | 0.028 (2) | 0.022 (3) | 0.0014 (19) | 0.005 (2) | 0.0001 (18) |
C16 | 0.032 (3) | 0.025 (2) | 0.023 (3) | 0.0024 (19) | 0.002 (2) | −0.0028 (18) |
C17 | 0.033 (3) | 0.057 (3) | 0.018 (3) | 0.000 (2) | 0.005 (2) | −0.003 (2) |
C18 | 0.035 (3) | 0.055 (3) | 0.028 (3) | 0.003 (2) | 0.009 (2) | −0.003 (2) |
C19 | 0.043 (3) | 0.055 (3) | 0.033 (3) | 0.001 (3) | 0.015 (3) | 0.000 (2) |
C20 | 0.037 (3) | 0.047 (3) | 0.026 (3) | −0.004 (2) | −0.006 (2) | −0.003 (2) |
C21 | 0.028 (3) | 0.045 (3) | 0.036 (3) | 0.006 (2) | 0.003 (2) | −0.002 (2) |
C22 | 0.027 (2) | 0.041 (2) | 0.031 (2) | −0.003 (2) | 0.0067 (19) | −0.005 (2) |
C23 | 0.0186 (16) | 0.042 (2) | 0.033 (2) | 0.002 (2) | −0.0011 (14) | 0.002 (2) |
C24 | 0.032 (2) | 0.041 (2) | 0.036 (3) | 0.002 (2) | 0.000 (2) | 0.002 (2) |
C25 | 0.037 (3) | 0.029 (2) | 0.046 (3) | 0.004 (2) | 0.001 (2) | −0.002 (2) |
C26 | 0.035 (3) | 0.041 (3) | 0.034 (3) | −0.001 (2) | 0.001 (2) | −0.011 (2) |
C27 | 0.024 (3) | 0.036 (3) | 0.037 (3) | 0.000 (2) | 0.005 (2) | −0.007 (2) |
N1 | 0.031 (2) | 0.037 (2) | 0.021 (2) | −0.0023 (18) | 0.0028 (19) | −0.0010 (17) |
N2 | 0.053 (3) | 0.042 (2) | 0.026 (2) | −0.005 (2) | 0.010 (2) | −0.004 (2) |
N3 | 0.034 (2) | 0.040 (2) | 0.024 (2) | 0.0030 (19) | 0.0038 (19) | −0.0017 (18) |
N4 | 0.049 (3) | 0.041 (2) | 0.021 (2) | 0.003 (2) | 0.009 (2) | −0.0004 (18) |
N5 | 0.033 (2) | 0.050 (3) | 0.046 (3) | 0.003 (2) | 0.005 (2) | −0.002 (2) |
O1 | 0.035 (2) | 0.0408 (17) | 0.039 (2) | −0.0036 (16) | 0.0040 (17) | 0.0008 (16) |
O2 | 0.066 (3) | 0.044 (2) | 0.0266 (19) | 0.0210 (19) | 0.0154 (18) | 0.0088 (17) |
O3 | 0.034 (2) | 0.050 (2) | 0.045 (2) | −0.0060 (18) | 0.0060 (18) | −0.0033 (19) |
O4 | 0.057 (3) | 0.045 (2) | 0.036 (2) | 0.0186 (18) | 0.0198 (18) | 0.0104 (17) |
O5 | 0.047 (3) | 0.051 (3) | 0.040 (3) | −0.0054 (17) | 0.008 (3) | −0.0061 (17) |
O6 | 0.087 (4) | 0.077 (3) | 0.045 (3) | −0.010 (3) | 0.009 (2) | −0.014 (2) |
O7 | 0.066 (3) | 0.049 (2) | 0.043 (3) | −0.008 (2) | 0.012 (2) | −0.0047 (19) |
O8 | 0.056 (4) | 0.063 (3) | 0.055 (4) | −0.009 (2) | 0.028 (3) | −0.015 (2) |
O9 | 0.055 (2) | 0.0404 (19) | 0.0336 (19) | 0.0007 (17) | 0.0046 (17) | −0.0005 (16) |
O10 | 0.049 (2) | 0.055 (2) | 0.031 (2) | −0.005 (2) | 0.0108 (18) | −0.0114 (18) |
O11 | 0.067 (4) | 0.061 (2) | 0.025 (2) | 0.005 (3) | 0.006 (2) | 0.003 (2) |
O12 | 0.054 (2) | 0.048 (2) | 0.035 (2) | 0.0018 (18) | 0.0044 (17) | −0.0097 (17) |
Co1—O4 | 2.151 (4) | C17—C20 | 1.402 (8) |
Co1—O2 | 2.160 (4) | C17—H17 | 0.9300 |
Co1—O3 | 2.199 (4) | C18—C19 | 1.384 (8) |
Co1—O1 | 2.200 (4) | C18—H18 | 0.9300 |
Co1—N1 | 2.279 (5) | C19—N4 | 1.323 (8) |
Co1—N3 | 2.271 (5) | C19—H19 | 0.9300 |
C1—N1 | 1.344 (7) | C20—N4 | 1.311 (8) |
C1—C4 | 1.388 (8) | C20—H20 | 0.9300 |
C1—H1 | 0.9300 | C21—O12 | 1.241 (7) |
C2—N1 | 1.326 (7) | C21—O11 | 1.274 (8) |
C2—C3 | 1.377 (8) | C21—C23 | 1.503 (11) |
C2—H2 | 0.9300 | C22—O9 | 1.237 (6) |
C3—C5 | 1.377 (7) | C22—O10 | 1.258 (6) |
C3—H3 | 0.9300 | C22—C27 | 1.529 (8) |
C4—C5 | 1.384 (7) | C23—C24 | 1.390 (7) |
C4—H4 | 0.9300 | C23—N5 | 1.416 (10) |
C5—C6 | 1.493 (6) | C24—C25 | 1.397 (8) |
C6—C7 | 1.392 (8) | C24—H24 | 0.9300 |
C6—C8 | 1.407 (8) | C25—C26 | 1.377 (8) |
C7—C10 | 1.380 (9) | C25—H25 | 0.9300 |
C7—H7 | 0.9300 | C26—C27 | 1.405 (7) |
C8—C9 | 1.381 (8) | C26—H26 | 0.9300 |
C8—H8 | 0.9300 | C27—N5 | 1.375 (8) |
C9—N2 | 1.346 (8) | O1—H1W | 0.82 (6) |
C9—H9 | 0.9300 | O1—H2W | 0.82 (3) |
C10—N2 | 1.329 (9) | O2—H3W | 0.80 (6) |
C10—H10 | 0.9300 | O2—H4W | 0.81 (3) |
C11—N3 | 1.351 (7) | O3—H5W | 0.82 (6) |
C11—C14 | 1.379 (8) | O3—H6W | 0.816 (11) |
C11—H11 | 0.9300 | O4—H7W | 0.82 (6) |
C12—N3 | 1.317 (8) | O4—H8W | 0.82 (5) |
C12—C13 | 1.383 (8) | O5—H9W | 0.81 (4) |
C12—H12 | 0.9300 | O5—H10W | 0.82 (7) |
C13—C15 | 1.413 (8) | O6—H11W | 0.82 (4) |
C13—H13 | 0.9300 | O6—H12W | 0.82 (3) |
C14—C15 | 1.380 (8) | O7—H13W | 0.82 (5) |
C14—H14 | 0.9300 | O7—H14W | 0.82 (3) |
C15—C16 | 1.482 (7) | O8—H15W | 0.82 (6) |
C16—C18 | 1.387 (8) | O8—H16W | 0.82 (4) |
C16—C17 | 1.393 (7) | ||
O4—Co1—O2 | 179.6 (2) | C18—C16—C15 | 122.0 (5) |
O4—Co1—O3 | 88.71 (17) | C17—C16—C15 | 120.7 (4) |
O2—Co1—O3 | 91.11 (18) | C16—C17—C20 | 118.7 (5) |
O4—Co1—O1 | 91.40 (17) | C16—C17—H17 | 120.6 |
O2—Co1—O1 | 88.77 (17) | C20—C17—H17 | 120.6 |
O3—Co1—O1 | 178.5 (2) | C19—C18—C16 | 118.4 (5) |
O4—Co1—N1 | 88.11 (16) | C19—C18—H18 | 120.8 |
O2—Co1—N1 | 91.48 (15) | C16—C18—H18 | 120.8 |
O3—Co1—N1 | 86.82 (17) | N4—C19—C18 | 125.0 (6) |
O1—Co1—N1 | 91.71 (16) | N4—C19—H19 | 117.6 |
O4—Co1—N3 | 91.27 (16) | C18—C19—H19 | 117.5 |
O2—Co1—N3 | 89.13 (16) | N4—C20—C17 | 123.9 (5) |
O3—Co1—N3 | 91.97 (17) | N4—C20—H20 | 118.0 |
O1—Co1—N3 | 89.49 (17) | C17—C20—H20 | 118.0 |
N1—Co1—N3 | 178.66 (19) | O12—C21—O11 | 124.3 (6) |
N1—C1—C4 | 123.2 (5) | O12—C21—C23 | 118.8 (5) |
N1—C1—H1 | 118.4 | O11—C21—C23 | 116.8 (5) |
C4—C1—H1 | 118.4 | O9—C22—O10 | 125.3 (5) |
N1—C2—C3 | 124.4 (6) | O9—C22—C27 | 116.9 (4) |
N1—C2—H2 | 117.8 | O10—C22—C27 | 117.7 (4) |
C3—C2—H2 | 117.8 | C24—C23—N5 | 117.7 (8) |
C2—C3—C5 | 119.4 (5) | C24—C23—C21 | 121.6 (7) |
C2—C3—H3 | 120.3 | N5—C23—C21 | 120.7 (4) |
C5—C3—H3 | 120.3 | C23—C24—C25 | 120.6 (7) |
C5—C4—C1 | 119.4 (5) | C23—C24—H24 | 119.7 |
C5—C4—H4 | 120.3 | C25—C24—H24 | 119.7 |
C1—C4—H4 | 120.3 | C26—C25—C24 | 120.6 (5) |
C3—C5—C4 | 117.3 (5) | C26—C25—H25 | 119.7 |
C3—C5—C6 | 121.0 (5) | C24—C25—H25 | 119.7 |
C4—C5—C6 | 121.7 (5) | C25—C26—C27 | 120.1 (5) |
C7—C6—C8 | 115.5 (5) | C25—C26—H26 | 119.9 |
C7—C6—C5 | 122.5 (5) | C27—C26—H26 | 119.9 |
C8—C6—C5 | 121.9 (5) | N5—C27—C26 | 118.9 (6) |
C10—C7—C6 | 120.0 (6) | N5—C27—C22 | 121.4 (4) |
C10—C7—H7 | 120.0 | C26—C27—C22 | 119.7 (5) |
C6—C7—H7 | 120.0 | C2—N1—C1 | 116.2 (5) |
C9—C8—C6 | 120.3 (6) | C2—N1—Co1 | 117.5 (4) |
C9—C8—H8 | 119.9 | C1—N1—Co1 | 124.9 (3) |
C6—C8—H8 | 119.8 | C10—N2—C9 | 115.8 (5) |
N2—C9—C8 | 123.6 (6) | C12—N3—C11 | 115.8 (5) |
N2—C9—H9 | 118.2 | C12—N3—Co1 | 124.3 (4) |
C8—C9—H9 | 118.2 | C11—N3—Co1 | 119.0 (4) |
N2—C10—C7 | 124.8 (6) | C20—N4—C19 | 116.6 (5) |
N2—C10—H10 | 117.6 | C27—N5—C23 | 122.1 (5) |
C7—C10—H10 | 117.6 | Co1—O1—H1W | 115 (5) |
N3—C11—C14 | 123.6 (5) | Co1—O1—H2W | 123 (5) |
N3—C11—H11 | 118.2 | H1W—O1—H2W | 115 (3) |
C14—C11—H11 | 118.2 | Co1—O2—H3W | 132 (5) |
N3—C12—C13 | 124.4 (5) | Co1—O2—H4W | 95 (5) |
N3—C12—H12 | 117.8 | H3W—O2—H4W | 120 (3) |
C13—C12—H12 | 117.8 | Co1—O3—H5W | 125 (5) |
C12—C13—C15 | 120.2 (5) | Co1—O3—H6W | 114 (5) |
C12—C13—H13 | 119.9 | H5W—O3—H6W | 114 (3) |
C15—C13—H13 | 119.9 | Co1—O4—H7W | 122 (4) |
C11—C14—C15 | 121.2 (5) | Co1—O4—H8W | 127 (4) |
C11—C14—H14 | 119.4 | H7W—O4—H8W | 111 (7) |
C15—C14—H14 | 119.4 | H9W—O5—H10W | 115 (7) |
C14—C15—C13 | 114.7 (5) | H11W—O6—H12W | 116 (7) |
C14—C15—C16 | 123.1 (4) | H13W—O7—H14W | 112 (3) |
C13—C15—C16 | 122.2 (5) | H15W—O8—H16W | 115 (3) |
C18—C16—C17 | 117.4 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1W···O10i | 0.82 (6) | 1.93 (6) | 2.728 (6) | 162 (7) |
O1—H2W···O5ii | 0.82 (3) | 1.96 (2) | 2.769 (6) | 169 (8) |
O2—H3W···O8iii | 0.80 (6) | 2.05 (6) | 2.843 (8) | 173 (8) |
O2—H4W···N2iv | 0.81 (3) | 2.06 (4) | 2.755 (6) | 145 (7) |
O3—H5W···O7 | 0.82 (6) | 1.95 (6) | 2.772 (6) | 176 (10) |
O3—H6W···O8v | 0.82 (1) | 2.01 (3) | 2.789 (7) | 161 (6) |
O4—H7W···O5 | 0.82 (6) | 2.06 (3) | 2.826 (7) | 155 (7) |
O4—H8W···N4v | 0.82 (5) | 2.00 (3) | 2.769 (6) | 155 (7) |
O5—H9W···O9i | 0.81 (4) | 2.00 (3) | 2.777 (7) | 161 (7) |
O5—H10W···O7vi | 0.82 (7) | 2.01 (6) | 2.822 (8) | 176 (7) |
O6—H11W···O12vii | 0.82 (4) | 2.16 (4) | 2.825 (6) | 137 (6) |
O7—H14W···O11 | 0.82 (3) | 1.82 (4) | 2.631 (7) | 174 (8) |
O8—H15W···O10 | 0.82 (6) | 1.96 (7) | 2.746 (8) | 162 (7) |
O8—H16W···O6viii | 0.82 (4) | 1.94 (4) | 2.747 (9) | 172 (8) |
O6—H12W···O11 | 0.82 (3) | 2.30 (5) | 2.933 (7) | 135 (7) |
Symmetry codes: (i) x+1/2, −y+3/2, z+1/2; (ii) x, y+1, z; (iii) x, −y+2, z+1/2; (iv) x, −y+2, z−1/2; (v) x, −y+1, z+1/2; (vi) x+1/2, y−1/2, z; (vii) x, y−1, z; (viii) x, −y+1, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [Co(C10H8N2)2(H2O)4](C7H3NO4)·4H2O |
Mr | 680.53 |
Crystal system, space group | Monoclinic, Cc |
Temperature (K) | 293 |
a, b, c (Å) | 18.1827 (5), 6.8537 (10), 25.1485 (5) |
β (°) | 99.398 (10) |
V (Å3) | 3091.9 (5) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.63 |
Crystal size (mm) | 0.42 × 0.28 × 0.22 |
Data collection | |
Diffractometer | Bruker APEXII CCD area-detector |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.779, 0.875 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5091, 3167, 2936 |
Rint | 0.033 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.043, 0.129, 1.00 |
No. of reflections | 3167 |
No. of parameters | 456 |
No. of restraints | 26 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.40, −0.58 |
Absolute structure | Flack (1983), with how many Friedel pairs? |
Absolute structure parameter | 0.65 (4) |
Computer programs: APEX2 (Bruker, 2004), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2001).
Co1—O4 | 2.151 (4) | Co1—O1 | 2.200 (4) |
Co1—O2 | 2.160 (4) | Co1—N1 | 2.279 (5) |
Co1—O3 | 2.199 (4) | Co1—N3 | 2.271 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1W···O10i | 0.82 (6) | 1.93 (6) | 2.728 (6) | 162 (7) |
O1—H2W···O5ii | 0.82 (3) | 1.96 (2) | 2.769 (6) | 169 (8) |
O2—H3W···O8iii | 0.80 (6) | 2.05 (6) | 2.843 (8) | 173 (8) |
O2—H4W···N2iv | 0.81 (3) | 2.06 (4) | 2.755 (6) | 145 (7) |
O3—H5W···O7 | 0.82 (6) | 1.95 (6) | 2.772 (6) | 176 (10) |
O3—H6W···O8v | 0.816 (11) | 2.01 (3) | 2.789 (7) | 161 (6) |
O4—H7W···O5 | 0.82 (6) | 2.06 (3) | 2.826 (7) | 155 (7) |
O4—H8W···N4v | 0.82 (5) | 2.00 (3) | 2.769 (6) | 155 (7) |
O5—H9W···O9i | 0.81 (4) | 2.00 (3) | 2.777 (7) | 161 (7) |
O5—H10W···O7vi | 0.82 (7) | 2.01 (6) | 2.822 (8) | 176 (7) |
O6—H11W···O12vii | 0.82 (4) | 2.16 (4) | 2.825 (6) | 137 (6) |
O7—H14W···O11 | 0.82 (3) | 1.82 (4) | 2.631 (7) | 174 (8) |
O8—H15W···O10 | 0.82 (6) | 1.96 (7) | 2.746 (8) | 162 (7) |
O8—H16W···O6viii | 0.82 (4) | 1.94 (4) | 2.747 (9) | 172 (8) |
O6—H12W···O11 | 0.82 (3) | 2.30 (5) | 2.933 (7) | 135 (7) |
Symmetry codes: (i) x+1/2, −y+3/2, z+1/2; (ii) x, y+1, z; (iii) x, −y+2, z+1/2; (iv) x, −y+2, z−1/2; (v) x, −y+1, z+1/2; (vi) x+1/2, y−1/2, z; (vii) x, y−1, z; (viii) x, −y+1, z−1/2. |
As part of our studies of coordination polymer networks (Howell et al., 2001), the molecular title compound, (I), arose.
The Coii atom is (I) is coordinated by two monodentate 4,4'-bipyridine molecules in the axial sites and four associated water molecules in the equatorial plane with the r.m.s. deviation for the fitted atoms (Co1, O1, O2, O3, O4) being 0.012 Å (Fig. 1, Table 1). The dihedral angle between the N1 and N2 rings is 6.2 (3)°; that between the N3 and N4 rings is 6.9 (3)°.
A network of O—H···O and O—H···N hydrogen bonds (Table 2, Fig. 2) helps to establish the packing for (I).