In the title compound, {[Co(C
7H
3NO
5)(C
13H
14N
2)(H
2O)]·2H
2O}
n, the Co
II atom is coordinated by two O atoms from a pyridine-2,6-dicarboxylate
N-oxide ligand, two N atoms from two 1,3-di-4-pyridylpropane ligands and one water molecule, and displays a distorted square-pyramidal coordination geometry. The 1,3-di-4-pyridylpropane ligands link the Co
II atoms into an infinite zigzag chain parallel to [010]. The chains are further linked through O—H

O and C—H

O hydrogen bonds, forming a three-dimensional supramolecular network.
Supporting information
CCDC reference: 709667
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean
(C-C) = 0.008 Å
- R factor = 0.059
- wR factor = 0.175
- Data-to-parameter ratio = 13.4
checkCIF/PLATON results
No syntax errors found
Alert level C
Value of measurement temperature given = 296.000
Value of melting point given = 0.000
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 -- O1W .. 6.05 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 -- N2 .. 6.00 su
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Co1
PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 8
PLAT417_ALERT_2_C Short Inter D-H..H-D H2W .. H4W .. 2.11 Ang.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
Alert level G
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 9
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
7 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
5 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
A mixture of cobalt chloride (0.238 g, 1 mmol), pyridine-2,6-dicarboxylic acid
N-oxide (0.181 g, 1 mmol), 1,3-di-4-pyridylpropane (0.198 g, 1 mmol), NaOH
(0.06 g, 1.5 mmol) and H2O (12 ml) was placed in a 23 ml Teflon-lined
reactor, which was heated to 433 K for 3 d and then cooled to room temperature
at a rate of 10 K h-1. The crystals obtained were washed with water and
dryed in air.
H atoms bound to C atoms were positioned geometrically and refined as riding
atoms, with C—H = 0.93(CH) and 0.97(CH2) Å and with Uiso(H) =
1.2Ueq(C). H atoms of water molecules were located on a difference
Fourier map and fixed in the refinements, with Uiso(H) =
1.5Ueq(O).
Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); 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 (Sheldrick, 2008).
catena-Poly[[[aqua(pyridine-2,6-dicarboxylato N-oxide-
κ2O1,
O2)cobalt(II)]-µ-1,3-di-4-pyridylpropane-
κ2N:
N'] dihydrate]
top
Crystal data top
[Co(C7H3NO5)(C13H14N2)(H2O)]·2H2O | F(000) = 1020 |
Mr = 492.34 | Dx = 1.509 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 5837 reflections |
a = 10.2712 (12) Å | θ = 2.8–27.9° |
b = 11.5251 (13) Å | µ = 0.84 mm−1 |
c = 18.309 (2) Å | T = 296 K |
β = 90.521 (2)° | Block, colorless |
V = 2167.3 (4) Å3 | 0.35 × 0.29 × 0.25 mm |
Z = 4 | |
Data collection top
Bruker SMART APEXII CCD area-detector diffractometer | 3897 independent reflections |
Radiation source: fine-focus sealed tube | 2170 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.064 |
ϕ and ω scans | θmax = 25.2°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −12→12 |
Tmin = 0.751, Tmax = 0.817 | k = −13→13 |
10818 measured reflections | l = −20→21 |
Refinement top
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)] = 0.059 | H-atom parameters constrained |
wR(F2) = 0.175 | w = 1/[σ2(Fo2) + (0.0828P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max < 0.001 |
3897 reflections | Δρmax = 0.66 e Å−3 |
290 parameters | Δρmin = −0.40 e Å−3 |
9 restraints | Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0030 (8) |
Crystal data top
[Co(C7H3NO5)(C13H14N2)(H2O)]·2H2O | V = 2167.3 (4) Å3 |
Mr = 492.34 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.2712 (12) Å | µ = 0.84 mm−1 |
b = 11.5251 (13) Å | T = 296 K |
c = 18.309 (2) Å | 0.35 × 0.29 × 0.25 mm |
β = 90.521 (2)° | |
Data collection top
Bruker SMART APEXII CCD area-detector diffractometer | 3897 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 2170 reflections with I > 2σ(I) |
Tmin = 0.751, Tmax = 0.817 | Rint = 0.064 |
10818 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.059 | 9 restraints |
wR(F2) = 0.175 | H-atom parameters constrained |
S = 1.00 | Δρmax = 0.66 e Å−3 |
3897 reflections | Δρmin = −0.40 e Å−3 |
290 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
O4 | 0.3287 (4) | −0.0221 (4) | 0.4108 (2) | 0.0776 (13) | |
N3 | 0.2102 (4) | 1.1756 (4) | 0.1902 (2) | 0.0519 (11) | |
C19 | 0.2965 (6) | 1.0894 (5) | 0.1927 (3) | 0.0622 (16) | |
H19 | 0.3729 | 1.1009 | 0.2194 | 0.075* | |
C20 | 0.2794 (6) | 0.9841 (5) | 0.1583 (3) | 0.0609 (15) | |
H20 | 0.3432 | 0.9272 | 0.1621 | 0.073* | |
C18 | 0.1003 (5) | 1.1549 (5) | 0.1514 (3) | 0.0568 (15) | |
H18 | 0.0376 | 1.2129 | 0.1486 | 0.068* | |
C17 | 0.0769 (6) | 1.0515 (5) | 0.1159 (3) | 0.0597 (15) | |
H17 | −0.0007 | 1.0411 | 0.0902 | 0.072* | |
C16 | 0.1677 (5) | 0.9631 (5) | 0.1180 (3) | 0.0565 (14) | |
C15 | 0.1470 (6) | 0.8479 (5) | 0.0794 (3) | 0.0647 (16) | |
H15A | 0.1842 | 0.8532 | 0.0310 | 0.078* | |
H15B | 0.1948 | 0.7885 | 0.1059 | 0.078* | |
Co1 | 0.24328 (6) | 0.32149 (5) | 0.24652 (3) | 0.0423 (3) | |
O5 | 0.2788 (4) | 0.2215 (3) | 0.32898 (19) | 0.0565 (10) | |
N2 | 0.1568 (4) | 0.4237 (4) | 0.1728 (2) | 0.0522 (11) | |
O2 | 0.2658 (5) | 0.5550 (4) | 0.4120 (2) | 0.0892 (15) | |
O1 | 0.2384 (4) | 0.4531 (3) | 0.3113 (2) | 0.0777 (13) | |
O3 | 0.4937 (4) | 0.0354 (3) | 0.3417 (2) | 0.0761 (12) | |
C6 | 0.3381 (5) | 0.3644 (5) | 0.4174 (3) | 0.0513 (14) | |
C12 | 0.1618 (6) | 0.5381 (5) | 0.0652 (3) | 0.0593 (15) | |
H12 | 0.2043 | 0.5575 | 0.0223 | 0.071* | |
N1 | 0.3424 (4) | 0.2545 (4) | 0.3900 (2) | 0.0494 (11) | |
C3 | 0.4691 (6) | 0.1910 (6) | 0.4901 (3) | 0.0702 (18) | |
H3 | 0.5156 | 0.1326 | 0.5137 | 0.084* | |
C7 | 0.2755 (6) | 0.4653 (5) | 0.3766 (3) | 0.0607 (15) | |
C2 | 0.4082 (5) | 0.1683 (5) | 0.4248 (3) | 0.0496 (13) | |
C13 | −0.0066 (6) | 0.6897 (4) | 0.0347 (3) | 0.0660 (17) | |
H13A | −0.0981 | 0.6750 | 0.0252 | 0.079* | |
H13B | 0.0381 | 0.6903 | −0.0117 | 0.079* | |
C10 | 0.0487 (5) | 0.5928 (5) | 0.0824 (3) | 0.0540 (14) | |
C1 | 0.4076 (6) | 0.0499 (5) | 0.3885 (3) | 0.0559 (14) | |
C5 | 0.3971 (6) | 0.3843 (5) | 0.4831 (3) | 0.0664 (16) | |
H5 | 0.3931 | 0.4585 | 0.5029 | 0.080* | |
C11 | 0.2145 (5) | 0.4541 (5) | 0.1107 (3) | 0.0547 (14) | |
H11 | 0.2918 | 0.4180 | 0.0976 | 0.066* | |
C8 | 0.0451 (6) | 0.4774 (5) | 0.1890 (3) | 0.0675 (17) | |
H8 | 0.0037 | 0.4577 | 0.2322 | 0.081* | |
C4 | 0.4619 (6) | 0.2997 (6) | 0.5211 (3) | 0.0730 (18) | |
H4 | 0.4999 | 0.3150 | 0.5663 | 0.088* | |
C9 | −0.0109 (6) | 0.5589 (5) | 0.1456 (3) | 0.0653 (16) | |
H9 | −0.0899 | 0.5918 | 0.1587 | 0.078* | |
C14 | 0.0088 (6) | 0.8095 (4) | 0.0717 (3) | 0.0641 (17) | |
H14A | −0.0387 | 0.8667 | 0.0432 | 0.077* | |
H14B | −0.0299 | 0.8064 | 0.1198 | 0.077* | |
O1W | 0.4465 (4) | 0.3311 (4) | 0.2130 (3) | 0.0969 (16) | |
H1W | 0.4767 | 0.3944 | 0.2011 | 0.145* | |
H2W | 0.4891 | 0.3034 | 0.2471 | 0.145* | |
O2W | 0.6417 (5) | 0.2145 (5) | 0.2840 (3) | 0.1170 (19) | |
H3W | 0.6669 | 0.1724 | 0.2494 | 0.175* | |
H4W | 0.5887 | 0.1753 | 0.3084 | 0.175* | |
O3W | 0.2003 (5) | 0.7719 (5) | 0.3494 (4) | 0.141 (2) | |
H5W | 0.2281 | 0.7061 | 0.3618 | 0.212* | |
H6W | 0.2190 | 0.8220 | 0.3795 | 0.212* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
O4 | 0.089 (3) | 0.053 (3) | 0.091 (3) | −0.012 (2) | 0.005 (2) | 0.013 (2) |
N3 | 0.058 (3) | 0.044 (3) | 0.053 (3) | 0.005 (2) | −0.012 (2) | 0.000 (2) |
C19 | 0.074 (4) | 0.043 (4) | 0.069 (4) | 0.008 (3) | −0.015 (3) | −0.002 (3) |
C20 | 0.066 (4) | 0.045 (4) | 0.071 (4) | 0.008 (3) | −0.010 (3) | −0.005 (3) |
C18 | 0.061 (4) | 0.038 (3) | 0.071 (4) | 0.006 (3) | −0.012 (3) | 0.002 (3) |
C17 | 0.070 (4) | 0.038 (3) | 0.071 (4) | −0.008 (3) | −0.014 (3) | −0.004 (3) |
C16 | 0.067 (4) | 0.043 (3) | 0.059 (3) | 0.003 (3) | −0.002 (3) | −0.003 (3) |
C15 | 0.080 (4) | 0.045 (4) | 0.069 (4) | −0.005 (3) | −0.003 (3) | −0.004 (3) |
Co1 | 0.0543 (5) | 0.0245 (4) | 0.0478 (4) | 0.0021 (3) | −0.0085 (3) | 0.0006 (3) |
O5 | 0.075 (3) | 0.040 (2) | 0.054 (2) | 0.0000 (19) | −0.0150 (19) | −0.0013 (18) |
N2 | 0.059 (3) | 0.042 (3) | 0.056 (3) | 0.001 (2) | −0.002 (2) | −0.003 (2) |
O2 | 0.133 (4) | 0.046 (3) | 0.088 (3) | 0.019 (3) | −0.033 (3) | −0.024 (2) |
O1 | 0.121 (4) | 0.039 (2) | 0.072 (3) | 0.010 (2) | −0.026 (3) | −0.005 (2) |
O3 | 0.074 (3) | 0.048 (3) | 0.107 (3) | 0.005 (2) | 0.022 (3) | −0.008 (2) |
C6 | 0.055 (3) | 0.040 (3) | 0.059 (3) | 0.007 (3) | −0.009 (3) | −0.008 (3) |
C12 | 0.080 (4) | 0.048 (4) | 0.050 (3) | −0.005 (3) | −0.001 (3) | 0.002 (3) |
N1 | 0.055 (3) | 0.040 (3) | 0.053 (3) | 0.001 (2) | −0.007 (2) | 0.002 (2) |
C3 | 0.076 (4) | 0.066 (5) | 0.068 (4) | 0.010 (3) | −0.018 (3) | 0.010 (3) |
C7 | 0.071 (4) | 0.045 (4) | 0.066 (4) | 0.009 (3) | −0.011 (3) | −0.013 (3) |
C2 | 0.050 (3) | 0.044 (3) | 0.055 (3) | 0.004 (3) | −0.001 (3) | 0.004 (3) |
C13 | 0.087 (4) | 0.042 (3) | 0.069 (4) | 0.003 (3) | −0.027 (3) | 0.003 (3) |
C10 | 0.059 (3) | 0.037 (3) | 0.066 (4) | 0.001 (3) | −0.013 (3) | −0.003 (3) |
C1 | 0.064 (4) | 0.041 (4) | 0.062 (4) | 0.007 (3) | −0.013 (3) | 0.008 (3) |
C5 | 0.086 (4) | 0.047 (4) | 0.066 (4) | 0.006 (3) | −0.014 (3) | −0.008 (3) |
C11 | 0.058 (3) | 0.048 (4) | 0.058 (3) | 0.008 (3) | 0.000 (3) | −0.003 (3) |
C8 | 0.068 (4) | 0.065 (4) | 0.070 (4) | 0.015 (3) | 0.008 (3) | 0.009 (3) |
C4 | 0.088 (5) | 0.065 (4) | 0.066 (4) | −0.001 (4) | −0.029 (3) | −0.004 (3) |
C9 | 0.068 (4) | 0.056 (4) | 0.072 (4) | 0.015 (3) | 0.006 (3) | 0.012 (3) |
C14 | 0.078 (4) | 0.033 (3) | 0.081 (4) | −0.004 (3) | −0.027 (3) | 0.005 (3) |
O1W | 0.074 (3) | 0.070 (3) | 0.147 (4) | −0.008 (2) | −0.002 (3) | 0.047 (3) |
O2W | 0.116 (4) | 0.098 (4) | 0.136 (5) | −0.009 (3) | −0.017 (3) | 0.034 (4) |
O3W | 0.115 (4) | 0.075 (4) | 0.233 (7) | −0.015 (3) | −0.046 (4) | 0.024 (4) |
Geometric parameters (Å, º) top
O4—C1 | 1.232 (7) | C12—C10 | 1.361 (7) |
N3—C19 | 1.332 (6) | C12—C11 | 1.384 (7) |
N3—C18 | 1.348 (6) | C12—H12 | 0.9300 |
N3—Co1i | 2.000 (4) | N1—C2 | 1.358 (6) |
C19—C20 | 1.378 (7) | C3—C2 | 1.370 (7) |
C19—H19 | 0.9300 | C3—C4 | 1.377 (8) |
C20—C16 | 1.379 (7) | C3—H3 | 0.9300 |
C20—H20 | 0.9300 | C2—C1 | 1.518 (7) |
C18—C17 | 1.378 (7) | C13—C10 | 1.524 (7) |
C18—H18 | 0.9300 | C13—C14 | 1.545 (7) |
C17—C16 | 1.381 (7) | C13—H13A | 0.9700 |
C17—H17 | 0.9300 | C13—H13B | 0.9700 |
C16—C15 | 1.519 (7) | C10—C9 | 1.371 (7) |
C15—C14 | 1.492 (7) | C5—C4 | 1.368 (8) |
C15—H15A | 0.9700 | C5—H5 | 0.9300 |
C15—H15B | 0.9700 | C11—H11 | 0.9300 |
Co1—O1 | 1.927 (4) | C8—C9 | 1.354 (7) |
Co1—O5 | 1.932 (3) | C8—H8 | 0.9300 |
Co1—N2 | 1.994 (4) | C4—H4 | 0.9300 |
Co1—N3ii | 2.000 (4) | C9—H9 | 0.9300 |
Co1—O1W | 2.184 (4) | C14—H14A | 0.9700 |
O5—N1 | 1.344 (5) | C14—H14B | 0.9700 |
N2—C11 | 1.334 (6) | O1W—H1W | 0.8200 |
N2—C8 | 1.339 (6) | O1W—H2W | 0.8200 |
O2—C7 | 1.224 (6) | O2W—H3W | 0.8400 |
O1—C7 | 1.259 (6) | O2W—H4W | 0.8400 |
O3—C1 | 1.248 (7) | O3W—H6W | 0.8200 |
C6—C5 | 1.361 (7) | O3W—H5W | 0.8400 |
C6—N1 | 1.363 (6) | O3W—H6W | 0.8200 |
C6—C7 | 1.522 (7) | | |
| | | |
C19—N3—C18 | 116.1 (5) | C2—C3—C4 | 120.5 (6) |
C19—N3—Co1i | 119.9 (4) | C2—C3—H3 | 119.7 |
C18—N3—Co1i | 123.9 (4) | C4—C3—H3 | 119.7 |
N3—C19—C20 | 123.9 (5) | O2—C7—O1 | 124.8 (6) |
N3—C19—H19 | 118.0 | O2—C7—C6 | 115.0 (5) |
C20—C19—H19 | 118.0 | O1—C7—C6 | 120.2 (5) |
C16—C20—C19 | 120.1 (5) | N1—C2—C3 | 119.4 (5) |
C16—C20—H20 | 119.9 | N1—C2—C1 | 116.9 (4) |
C19—C20—H20 | 119.9 | C3—C2—C1 | 123.7 (5) |
N3—C18—C17 | 122.9 (5) | C10—C13—C14 | 111.6 (4) |
N3—C18—H18 | 118.5 | C10—C13—H13A | 109.3 |
C17—C18—H18 | 118.5 | C14—C13—H13A | 109.3 |
C18—C17—C16 | 120.6 (5) | C10—C13—H13B | 109.3 |
C18—C17—H17 | 119.7 | C14—C13—H13B | 109.3 |
C16—C17—H17 | 119.7 | H13A—C13—H13B | 108.0 |
C20—C16—C17 | 116.3 (5) | C12—C10—C9 | 116.8 (5) |
C20—C16—C15 | 121.0 (5) | C12—C10—C13 | 121.4 (5) |
C17—C16—C15 | 122.7 (5) | C9—C10—C13 | 121.8 (5) |
C14—C15—C16 | 115.6 (5) | O4—C1—O3 | 127.6 (6) |
C14—C15—H15A | 108 | O4—C1—C2 | 117.4 (6) |
C16—C15—H15A | 108 | O3—C1—C2 | 114.9 (5) |
C14—C15—H15B | 108 | C6—C5—C4 | 122.7 (6) |
C16—C15—H15B | 108 | C6—C5—H5 | 118.7 |
H15A—C15—H15B | 107 | C4—C5—H5 | 118.7 |
O1—Co1—O5 | 89.67 (16) | N2—C11—C12 | 121.5 (5) |
O1—Co1—N2 | 86.43 (16) | N2—C11—H11 | 119.3 |
O5—Co1—N2 | 164.02 (17) | C12—C11—H11 | 119.3 |
O1—Co1—N3ii | 166.97 (19) | N2—C8—C9 | 123.4 (6) |
O5—Co1—N3ii | 86.08 (16) | N2—C8—H8 | 118.3 |
N2—Co1—N3ii | 94.30 (16) | C9—C8—H8 | 118.3 |
O1—Co1—O1W | 99.39 (19) | C5—C4—C3 | 117.8 (5) |
O5—Co1—O1W | 94.32 (16) | C5—C4—H4 | 121.1 |
N2—Co1—O1W | 101.61 (17) | C3—C4—H4 | 121.1 |
N3ii—Co1—O1W | 93.21 (18) | C8—C9—C10 | 120.2 (6) |
N1—O5—Co1 | 124.5 (3) | C8—C9—H9 | 119.9 |
C11—N2—C8 | 117.0 (5) | C10—C9—H9 | 119.9 |
C11—N2—Co1 | 122.3 (4) | C15—C14—C13 | 113.6 (5) |
C8—N2—Co1 | 120.1 (4) | C15—C14—H14A | 108.9 |
C7—O1—Co1 | 131.5 (4) | C13—C14—H14A | 108.9 |
C5—C6—N1 | 117.8 (5) | C15—C14—H14B | 108.9 |
C5—C6—C7 | 119.1 (5) | C13—C14—H14B | 108.9 |
N1—C6—C7 | 123.0 (4) | H14A—C14—H14B | 107.7 |
C10—C12—C11 | 121.0 (5) | Co1—O1W—H1W | 118.8 |
C10—C12—H12 | 119.5 | Co1—O1W—H2W | 105.7 |
C11—C12—H12 | 119.5 | H1W—O1W—H2W | 110 |
O5—N1—C2 | 114.7 (4) | H3W—O2W—H4W | 107 |
O5—N1—C6 | 123.5 (4) | H5W—O3W—H6W | 112 |
C2—N1—C6 | 121.7 (4) | | |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O3iii | 0.82 | 1.83 | 2.635 (5) | 165 |
O1W—H2W···O2W | 0.82 | 1.99 | 2.732 (6) | 150 |
O2W—H3W···O3Wiv | 0.84 | 2.55 | 3.018 (9) | 117 |
O2W—H4W···O3 | 0.84 | 1.98 | 2.778 (6) | 157 |
O3W—H5W···O2 | 0.84 | 2.01 | 2.828 (7) | 166 |
O3W—H6W···O4i | 0.82 | 2.19 | 2.935 (7) | 150 |
C3—H3···O4v | 0.93 | 2.46 | 3.364 (8) | 165 |
C9—H9···O5vi | 0.93 | 2.46 | 3.366 (7) | 164 |
C15—H15A···O2vii | 0.97 | 2.57 | 3.492 (7) | 159 |
C18—H18···O3Wvi | 0.93 | 2.55 | 3.369 (7) | 149 |
Symmetry codes: (i) x, y+1, z; (iii) −x+1, y+1/2, −z+1/2; (iv) −x+1, y−1/2, −z+1/2; (v) −x+1, −y, −z+1; (vi) −x, y+1/2, −z+1/2; (vii) x, −y+3/2, z−1/2. |
Experimental details
Crystal data |
Chemical formula | [Co(C7H3NO5)(C13H14N2)(H2O)]·2H2O |
Mr | 492.34 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 296 |
a, b, c (Å) | 10.2712 (12), 11.5251 (13), 18.309 (2) |
β (°) | 90.521 (2) |
V (Å3) | 2167.3 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.84 |
Crystal size (mm) | 0.35 × 0.29 × 0.25 |
|
Data collection |
Diffractometer | Bruker SMART APEXII CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.751, 0.817 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10818, 3897, 2170 |
Rint | 0.064 |
(sin θ/λ)max (Å−1) | 0.599 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.059, 0.175, 1.00 |
No. of reflections | 3897 |
No. of parameters | 290 |
No. of restraints | 9 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.66, −0.40 |
Selected bond lengths (Å) topCo1—O1 | 1.927 (4) | Co1—N3i | 2.000 (4) |
Co1—O5 | 1.932 (3) | Co1—O1W | 2.184 (4) |
Co1—N2 | 1.994 (4) | | |
Symmetry code: (i) x, y−1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O3ii | 0.82 | 1.83 | 2.635 (5) | 165 |
O1W—H2W···O2W | 0.82 | 1.99 | 2.732 (6) | 150 |
O2W—H3W···O3Wiii | 0.84 | 2.55 | 3.018 (9) | 117 |
O2W—H4W···O3 | 0.84 | 1.98 | 2.778 (6) | 157 |
O3W—H5W···O2 | 0.84 | 2.01 | 2.828 (7) | 166 |
O3W—H6W···O4iv | 0.82 | 2.19 | 2.935 (7) | 150 |
C3—H3···O4v | 0.93 | 2.46 | 3.364 (8) | 165 |
C9—H9···O5vi | 0.93 | 2.46 | 3.366 (7) | 164 |
C15—H15A···O2vii | 0.97 | 2.57 | 3.492 (7) | 159 |
C18—H18···O3Wvi | 0.93 | 2.55 | 3.369 (7) | 149 |
Symmetry codes: (ii) −x+1, y+1/2, −z+1/2; (iii) −x+1, y−1/2, −z+1/2; (iv) x, y+1, z; (v) −x+1, −y, −z+1; (vi) −x, y+1/2, −z+1/2; (vii) x, −y+3/2, z−1/2. |
In the structural investigation of metal complexes with pyridine-2,6-dicarboxylate-N-oxide (pdco), it has been found that pdco functions as a multidentate ligand with versatile coordination modes (Nathan et al., 1985; Wen et al., 2005, 2006; Wu et al., 2007). As is well known, 1,3-di-4-pyridylpropane may act in bidentate bridging or monodentate terminal modes, leading to the formation of one-, two- or three-dimensional network (Konar et al., 2003; Lai & Tiekink, 2004; Li et al., 2004). On the basis of these observations, we utilize pdco, 1,3-di-4-pyridylpropane and CoII ion as building blocks. A new one-dimensional coordination framework has been obtained from the hydrothermal treatment in an alkaline aqueous solution.
As illustrated in Fig. 1, the CoII atom exists in a distorted square-pyramidal environment, defined by two O atoms from one pdco ligand, two N atoms from two 1,3-di-4-pyridylpropane ligands and one water molecule (Table 1). The O1, O5, N2, N3i atoms (i = x, -1 + y, z) in the basal plane are alomst coplanar, and a water molecule lies at the apical position. The 1,3-di-4-pyridylpropane ligand in a bidentate bridging mode links the CoII atoms into an infinite zigzag chain, with the shortest Co···Co separation of 11.525 (3)Å and a Co—C13—Coii angle (ii = x, 1 + y, z) of 100.06 (4)°. The chains are further self-assembled into a three-dimensional supramolecular network through O—H···O and C—H···O hydrogen bonds (Table 2; Fig. 2).