Related literature
For a related structure, see Manna et al. (2005
).
Experimental
Data collection
Bruker SMART 1K CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 2004 ) Tmin = 0.891, Tmax = 0.954 8438 measured reflections 2726 independent reflections 2167 reflections with I > 2σ(I) Rint = 0.068
|
D—H⋯A | D—H | H⋯A | D⋯A | D—H⋯A | O3—H3A⋯N2i | 0.93 | 1.90 | 2.820 (5) | 171 | O3—H3B⋯O2ii | 1.03 | 1.71 | 2.704 (4) | 161 | Symmetry codes: (i) ; (ii) -x, -y, -z. | |
Data collection: SMART (Bruker, 2001
); cell refinement: SAINT (Bruker, 2001
); data reduction: SAINT; 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 and local programs.
Supporting information
CoCl2(1.0 mmol), terephthalic acid (1 mmol), and 4,4'-trimethylenedipyridine (1 mmol) were dissolved in water (10 ml). The solution was heated in a 25 ml Teflon lined reaction vessel at 433 K for ca 3 days and then cooled to room temperature. Purple crystals were obtained in a yield of 65%.
All non-water H atoms were positioned geometrically and refined by using a riding model with C—H = 0.93–0.96 Å and with Uiso(H) = 1.2 times Ueq(C), the water H atoms are firstly found, then refined freely.
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); 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) and local programs.
catena-Poly[[diaqua(4,4'-trimethylenedipyridine-
κN)cobalt(II)]- µ-terephthalato-
κ2O1:
O4]
top Crystal data top [Co(C8H4O4)(C13H14N2)2(H2O)2] | F(000) = 686 |
Mr = 655.60 | Dx = 1.369 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 11.232 (2) Å | Cell parameters from 3657 reflections |
b = 9.3784 (19) Å | θ = 1.4–27.9° |
c = 15.182 (3) Å | µ = 0.59 mm−1 |
β = 96.19 (3)° | T = 293 K |
V = 1589.9 (5) Å3 | Block, purple |
Z = 2 | 0.20 × 0.14 × 0.08 mm |
Data collection top Bruker SMART 1K CCD area-detector diffractometer | 2726 independent reflections |
Radiation source: sealed tube | 2167 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.068 |
Detector resolution: 8.192 pixels mm-1 | θmax = 25.0°, θmin = 1.8° |
Thin–slice ω scans | h = −11→13 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2004) | k = −8→11 |
Tmin = 0.891, Tmax = 0.954 | l = −17→18 |
8438 measured reflections | |
Refinement top Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.070 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.179 | H-atom parameters constrained |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0794P)2 + 1.059P] where P = (Fo2 + 2Fc2)/3 |
2726 reflections | (Δ/σ)max < 0.001 |
207 parameters | Δρmax = 1.05 e Å−3 |
0 restraints | Δρmin = −0.62 e Å−3 |
Crystal data top [Co(C8H4O4)(C13H14N2)2(H2O)2] | V = 1589.9 (5) Å3 |
Mr = 655.60 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 11.232 (2) Å | µ = 0.59 mm−1 |
b = 9.3784 (19) Å | T = 293 K |
c = 15.182 (3) Å | 0.20 × 0.14 × 0.08 mm |
β = 96.19 (3)° | |
Data collection top Bruker SMART 1K CCD area-detector diffractometer | 2726 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2004) | 2167 reflections with I > 2σ(I) |
Tmin = 0.891, Tmax = 0.954 | Rint = 0.068 |
8438 measured reflections | |
Refinement top R[F2 > 2σ(F2)] = 0.070 | 0 restraints |
wR(F2) = 0.179 | H-atom parameters constrained |
S = 1.13 | Δρmax = 1.05 e Å−3 |
2726 reflections | Δρmin = −0.62 e Å−3 |
207 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | 0.0000 | 0.0000 | 0.0000 | 0.0323 (3) | |
O1 | 0.1776 (3) | −0.0428 (3) | −0.0026 (2) | 0.0398 (8) | |
O2 | 0.2160 (3) | −0.0377 (4) | −0.1445 (2) | 0.0560 (10) | |
O3 | 0.0130 (3) | −0.0481 (3) | 0.1394 (2) | 0.0409 (8) | |
N1 | 0.0522 (3) | 0.2209 (4) | 0.0279 (2) | 0.0369 (9) | |
N2 | 0.7841 (4) | 0.5278 (5) | 0.2442 (3) | 0.0562 (12) | |
C1 | 0.0265 (4) | 0.2912 (5) | 0.1005 (3) | 0.0451 (11) | |
H1 | −0.0263 | 0.2493 | 0.1359 | 0.054* | |
C2 | 0.0747 (4) | 0.4234 (5) | 0.1253 (3) | 0.0479 (12) | |
H2 | 0.0544 | 0.4674 | 0.1765 | 0.057* | |
C3 | 0.1530 (4) | 0.4901 (5) | 0.0739 (3) | 0.0378 (10) | |
C4 | 0.1764 (4) | 0.4190 (5) | −0.0026 (3) | 0.0443 (11) | |
H4 | 0.2263 | 0.4604 | −0.0405 | 0.053* | |
C5 | 0.1259 (4) | 0.2869 (5) | −0.0226 (3) | 0.0449 (12) | |
H5 | 0.1441 | 0.2415 | −0.0739 | 0.054* | |
C6 | 0.2111 (4) | 0.6317 (5) | 0.1003 (4) | 0.0541 (14) | |
H6A | 0.1600 | 0.6837 | 0.1367 | 0.065* | |
H6B | 0.2183 | 0.6877 | 0.0474 | 0.065* | |
C7 | 0.3359 (4) | 0.6137 (5) | 0.1519 (4) | 0.0544 (14) | |
H7A | 0.3618 | 0.7056 | 0.1764 | 0.065* | |
H7B | 0.3290 | 0.5496 | 0.2013 | 0.065* | |
C8 | 0.4310 (5) | 0.5574 (6) | 0.0989 (4) | 0.0612 (15) | |
H8A | 0.4361 | 0.6191 | 0.0482 | 0.073* | |
H8B | 0.4073 | 0.4634 | 0.0767 | 0.073* | |
C9 | 0.5539 (4) | 0.5470 (5) | 0.1508 (3) | 0.0436 (11) | |
C10 | 0.6121 (4) | 0.4186 (5) | 0.1644 (4) | 0.0516 (13) | |
H10 | 0.5755 | 0.3347 | 0.1429 | 0.062* | |
H3B | −0.0679 | −0.0089 | 0.1545 | 0.09 (2)* | |
H3A | 0.0837 | −0.0307 | 0.1753 | 0.10 (2)* | |
C11 | 0.7261 (4) | 0.4149 (6) | 0.2103 (4) | 0.0553 (14) | |
H11 | 0.7639 | 0.3268 | 0.2176 | 0.066* | |
C12 | 0.6140 (5) | 0.6664 (6) | 0.1852 (4) | 0.0579 (14) | |
H12 | 0.5787 | 0.7559 | 0.1780 | 0.070* | |
C13 | 0.7273 (5) | 0.6521 (6) | 0.2307 (4) | 0.0602 (15) | |
H13 | 0.7660 | 0.7341 | 0.2531 | 0.072* | |
C14 | 0.2472 (4) | −0.0357 (4) | −0.0632 (3) | 0.0364 (10) | |
C15 | 0.3786 (3) | −0.0193 (4) | −0.0300 (3) | 0.0314 (9) | |
C16 | 0.4142 (4) | 0.0107 (4) | 0.0580 (3) | 0.0365 (10) | |
H16 | 0.3566 | 0.0188 | 0.0974 | 0.044* | |
C17 | 0.4659 (4) | −0.0292 (4) | −0.0888 (3) | 0.0366 (10) | |
H17 | 0.4436 | −0.0482 | −0.1484 | 0.044* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0153 (5) | 0.0487 (5) | 0.0327 (5) | −0.0044 (3) | 0.0010 (3) | 0.0013 (3) |
O1 | 0.0221 (16) | 0.0495 (18) | 0.048 (2) | −0.0006 (12) | 0.0036 (14) | 0.0055 (13) |
O2 | 0.0219 (18) | 0.099 (3) | 0.046 (2) | −0.0012 (16) | 0.0005 (15) | −0.0105 (18) |
O3 | 0.0268 (17) | 0.0538 (19) | 0.041 (2) | −0.0043 (13) | −0.0021 (14) | 0.0020 (14) |
N1 | 0.028 (2) | 0.041 (2) | 0.042 (2) | −0.0028 (15) | 0.0054 (16) | −0.0006 (16) |
N2 | 0.033 (2) | 0.089 (4) | 0.046 (3) | 0.002 (2) | −0.0009 (19) | 0.011 (2) |
C1 | 0.035 (3) | 0.054 (3) | 0.047 (3) | −0.003 (2) | 0.009 (2) | −0.001 (2) |
C2 | 0.041 (3) | 0.058 (3) | 0.044 (3) | 0.004 (2) | 0.000 (2) | −0.009 (2) |
C3 | 0.024 (2) | 0.043 (2) | 0.044 (3) | 0.0035 (18) | −0.0083 (18) | −0.001 (2) |
C4 | 0.036 (3) | 0.048 (3) | 0.049 (3) | −0.011 (2) | 0.003 (2) | 0.003 (2) |
C5 | 0.038 (3) | 0.049 (3) | 0.049 (3) | −0.009 (2) | 0.008 (2) | 0.000 (2) |
C6 | 0.034 (3) | 0.048 (3) | 0.077 (4) | 0.000 (2) | −0.009 (2) | −0.011 (2) |
C7 | 0.037 (3) | 0.056 (3) | 0.068 (4) | 0.001 (2) | −0.006 (2) | −0.019 (3) |
C8 | 0.039 (3) | 0.078 (4) | 0.062 (4) | 0.001 (3) | −0.012 (3) | −0.014 (3) |
C9 | 0.032 (3) | 0.053 (3) | 0.045 (3) | 0.003 (2) | −0.002 (2) | −0.002 (2) |
C10 | 0.044 (3) | 0.049 (3) | 0.062 (4) | −0.006 (2) | 0.006 (2) | 0.007 (2) |
C11 | 0.041 (3) | 0.064 (4) | 0.062 (4) | 0.012 (3) | 0.009 (3) | 0.022 (3) |
C12 | 0.046 (3) | 0.054 (3) | 0.071 (4) | 0.004 (2) | −0.009 (3) | −0.005 (3) |
C13 | 0.045 (3) | 0.069 (4) | 0.064 (4) | −0.016 (3) | −0.008 (3) | −0.006 (3) |
C14 | 0.020 (2) | 0.043 (3) | 0.046 (3) | −0.0023 (17) | 0.0015 (19) | 0.0016 (19) |
C15 | 0.018 (2) | 0.037 (2) | 0.039 (3) | 0.0000 (16) | 0.0010 (17) | −0.0018 (17) |
C16 | 0.018 (2) | 0.054 (3) | 0.039 (3) | −0.0029 (18) | 0.0095 (18) | −0.0022 (19) |
C17 | 0.023 (2) | 0.046 (3) | 0.040 (3) | −0.0013 (17) | 0.0032 (18) | −0.0042 (18) |
Geometric parameters (Å, º) top Co1—O1i | 2.039 (3) | C6—H6A | 0.9700 |
Co1—O1 | 2.039 (3) | C6—H6B | 0.9700 |
Co1—O3i | 2.154 (3) | C7—C8 | 1.500 (7) |
Co1—O3 | 2.154 (3) | C7—H7A | 0.9700 |
Co1—N1i | 2.183 (3) | C7—H7B | 0.9700 |
Co1—N1 | 2.183 (3) | C8—C9 | 1.517 (7) |
O1—C14 | 1.271 (5) | C8—H8A | 0.9700 |
O2—C14 | 1.247 (6) | C8—H8B | 0.9700 |
O3—H3B | 1.0283 | C9—C10 | 1.375 (7) |
O3—H3A | 0.9271 | C9—C12 | 1.381 (7) |
N1—C5 | 1.339 (5) | C10—C11 | 1.390 (7) |
N1—C1 | 1.342 (6) | C10—H10 | 0.9300 |
N2—C11 | 1.318 (7) | C11—H11 | 0.9300 |
N2—C13 | 1.334 (7) | C12—C13 | 1.388 (7) |
C1—C2 | 1.389 (7) | C12—H12 | 0.9300 |
C1—H1 | 0.9300 | C13—H13 | 0.9300 |
C2—C3 | 1.386 (7) | C14—C15 | 1.515 (6) |
C2—H2 | 0.9300 | C15—C16 | 1.381 (6) |
C3—C4 | 1.388 (6) | C15—C17 | 1.398 (6) |
C3—C6 | 1.515 (6) | C16—C17ii | 1.389 (6) |
C4—C5 | 1.383 (6) | C16—H16 | 0.9300 |
C4—H4 | 0.9300 | C17—C16ii | 1.389 (6) |
C5—H5 | 0.9300 | C17—H17 | 0.9300 |
C6—C7 | 1.540 (7) | | |
| | | |
O1i—Co1—O1 | 180.00 (16) | C7—C6—H6B | 109.1 |
O1i—Co1—O3i | 90.88 (12) | H6A—C6—H6B | 107.9 |
O1—Co1—O3i | 89.12 (12) | C8—C7—C6 | 115.3 (5) |
O1i—Co1—O3 | 89.12 (12) | C8—C7—H7A | 108.5 |
O1—Co1—O3 | 90.88 (12) | C6—C7—H7A | 108.5 |
O3i—Co1—O3 | 180.00 (16) | C8—C7—H7B | 108.5 |
O1i—Co1—N1i | 86.99 (12) | C6—C7—H7B | 108.5 |
O1—Co1—N1i | 93.01 (12) | H7A—C7—H7B | 107.5 |
O3i—Co1—N1i | 91.14 (12) | C7—C8—C9 | 113.9 (4) |
O3—Co1—N1i | 88.86 (12) | C7—C8—H8A | 108.8 |
O1i—Co1—N1 | 93.01 (12) | C9—C8—H8A | 108.8 |
O1—Co1—N1 | 86.99 (12) | C7—C8—H8B | 108.8 |
O3i—Co1—N1 | 88.86 (12) | C9—C8—H8B | 108.8 |
O3—Co1—N1 | 91.14 (12) | H8A—C8—H8B | 107.7 |
N1i—Co1—N1 | 180.0 (2) | C10—C9—C12 | 116.7 (5) |
C14—O1—Co1 | 133.1 (3) | C10—C9—C8 | 121.7 (4) |
Co1—O3—H3B | 100.2 | C12—C9—C8 | 121.6 (4) |
Co1—O3—H3A | 120.2 | C9—C10—C11 | 119.6 (5) |
H3B—O3—H3A | 121.8 | C9—C10—H10 | 120.2 |
C5—N1—C1 | 116.4 (4) | C11—C10—H10 | 120.2 |
C5—N1—Co1 | 119.8 (3) | N2—C11—C10 | 124.4 (5) |
C1—N1—Co1 | 123.3 (3) | N2—C11—H11 | 117.8 |
C11—N2—C13 | 115.7 (4) | C10—C11—H11 | 117.8 |
N1—C1—C2 | 123.3 (4) | C9—C12—C13 | 119.6 (5) |
N1—C1—H1 | 118.4 | C9—C12—H12 | 120.2 |
C2—C1—H1 | 118.4 | C13—C12—H12 | 120.2 |
C3—C2—C1 | 120.2 (4) | N2—C13—C12 | 124.0 (5) |
C3—C2—H2 | 119.9 | N2—C13—H13 | 118.0 |
C1—C2—H2 | 119.9 | C12—C13—H13 | 118.0 |
C2—C3—C4 | 116.3 (4) | O2—C14—O1 | 125.9 (4) |
C2—C3—C6 | 121.9 (4) | O2—C14—C15 | 119.4 (4) |
C4—C3—C6 | 121.8 (4) | O1—C14—C15 | 114.7 (4) |
C5—C4—C3 | 120.2 (4) | C16—C15—C17 | 118.8 (4) |
C5—C4—H4 | 119.9 | C16—C15—C14 | 120.8 (4) |
C3—C4—H4 | 119.9 | C17—C15—C14 | 120.4 (4) |
N1—C5—C4 | 123.5 (4) | C15—C16—C17ii | 121.3 (4) |
N1—C5—H5 | 118.2 | C15—C16—H16 | 119.3 |
C4—C5—H5 | 118.2 | C17ii—C16—H16 | 119.3 |
C3—C6—C7 | 112.4 (4) | C16ii—C17—C15 | 119.9 (4) |
C3—C6—H6A | 109.1 | C16ii—C17—H17 | 120.1 |
C7—C6—H6A | 109.1 | C15—C17—H17 | 120.1 |
C3—C6—H6B | 109.1 | | |
| | | |
O1i—Co1—O1—C14 | −175 (95) | C2—C3—C6—C7 | 94.5 (5) |
O3i—Co1—O1—C14 | 2.6 (4) | C4—C3—C6—C7 | −84.7 (6) |
O3—Co1—O1—C14 | −177.4 (4) | C3—C6—C7—C8 | 68.8 (6) |
N1i—Co1—O1—C14 | 93.7 (4) | C6—C7—C8—C9 | 177.5 (4) |
N1—Co1—O1—C14 | −86.3 (4) | C7—C8—C9—C10 | 118.4 (5) |
O1i—Co1—N1—C5 | −130.3 (3) | C7—C8—C9—C12 | −62.9 (7) |
O1—Co1—N1—C5 | 49.7 (3) | C12—C9—C10—C11 | −0.5 (7) |
O3i—Co1—N1—C5 | −39.5 (3) | C8—C9—C10—C11 | 178.3 (5) |
O3—Co1—N1—C5 | 140.5 (3) | C13—N2—C11—C10 | −1.2 (8) |
N1i—Co1—N1—C5 | 82 (48) | C9—C10—C11—N2 | 1.1 (8) |
O1i—Co1—N1—C1 | 58.2 (4) | C10—C9—C12—C13 | 0.0 (8) |
O1—Co1—N1—C1 | −121.8 (4) | C8—C9—C12—C13 | −178.7 (5) |
O3i—Co1—N1—C1 | 149.1 (4) | C11—N2—C13—C12 | 0.7 (8) |
O3—Co1—N1—C1 | −30.9 (4) | C9—C12—C13—N2 | −0.2 (9) |
N1i—Co1—N1—C1 | −90 (48) | Co1—O1—C14—O2 | −21.8 (7) |
C5—N1—C1—C2 | −1.9 (7) | Co1—O1—C14—C15 | 156.4 (3) |
Co1—N1—C1—C2 | 169.9 (3) | O2—C14—C15—C16 | 167.4 (4) |
N1—C1—C2—C3 | 0.5 (7) | O1—C14—C15—C16 | −10.9 (6) |
C1—C2—C3—C4 | 1.5 (7) | O2—C14—C15—C17 | −10.2 (6) |
C1—C2—C3—C6 | −177.7 (4) | O1—C14—C15—C17 | 171.5 (4) |
C2—C3—C4—C5 | −2.1 (7) | C17—C15—C16—C17ii | −0.8 (7) |
C6—C3—C4—C5 | 177.1 (4) | C14—C15—C16—C17ii | −178.5 (4) |
C1—N1—C5—C4 | 1.2 (7) | C16—C15—C17—C16ii | 0.8 (7) |
Co1—N1—C5—C4 | −170.8 (4) | C14—C15—C17—C16ii | 178.5 (4) |
C3—C4—C5—N1 | 0.8 (7) | | |
Symmetry codes: (i) −x, −y, −z; (ii) −x+1, −y, −z. |
Hydrogen-bond geometry (Å, º) top D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3A···N2iii | 0.93 | 1.90 | 2.820 (5) | 171 |
O3—H3B···O2i | 1.03 | 1.71 | 2.704 (4) | 161 |
Symmetry codes: (i) −x, −y, −z; (iii) −x+1, y−1/2, −z+1/2. |
Experimental details
Crystal data |
Chemical formula | [Co(C8H4O4)(C13H14N2)2(H2O)2] |
Mr | 655.60 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 11.232 (2), 9.3784 (19), 15.182 (3) |
β (°) | 96.19 (3) |
V (Å3) | 1589.9 (5) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.59 |
Crystal size (mm) | 0.20 × 0.14 × 0.08 |
|
Data collection |
Diffractometer | Bruker SMART 1K CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2004) |
Tmin, Tmax | 0.891, 0.954 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8438, 2726, 2167 |
Rint | 0.068 |
(sin θ/λ)max (Å−1) | 0.594 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.070, 0.179, 1.13 |
No. of reflections | 2726 |
No. of parameters | 207 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.05, −0.62 |
Hydrogen-bond geometry (Å, º) top D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3A···N2i | 0.93 | 1.90 | 2.820 (5) | 171.4 |
O3—H3B···O2ii | 1.03 | 1.71 | 2.704 (4) | 160.9 |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x, −y, −z. |
References
Bruker (2001). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Manna, S. C., Konar, S., Zangrando, E., Okamoto, K., Ribas, J. & Chaudhuri, N. R. (2005). Eur. J. Inorg. Chem. pp. 4646–4654. Web of Science CSD CrossRef Google Scholar
Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
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Co is six-coordinated by two terephthalate O atoms, two N atoms of 4,4'-trimethylenedipyridines and two water molecules in a distorted octahedral fashion. The Co—O and Co—N bond lengthes are in the normal range. The 4,4'-trimethylenedipyridine and terephthalate ligands adopt bidentate coordinated modes. As shown in Fig. 2, a chain structure is formed. These chains are further linked by O—H···O and O—H···N hydrogen bonds to generate a three-dimensional network.