Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807058333/hy2098sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807058333/hy2098Isup2.hkl |
CCDC reference: 672701
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.003 Å
- R factor = 0.041
- wR factor = 0.123
- Data-to-parameter ratio = 15.3
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 3000 Deg. PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.23
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Co1 (3) 1.76
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 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 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For general background, see: Wang et al. (2005). For related structures, see: Hao et al. (2005).
The title compound was prepared by a hydrothermal method. A mixture of Co(NO3)2.6H2O (0.115 g, 0.5 mmol), biphenyl-3,3',4,4'-tetracarboxylic acid (0.165 g, 0.5 mmol), 4,4'-bipyridine (0.125 g, 0.8 mmol) and water (10 ml) was stirred for 20 min and then transferred to a 23 ml Teflon-lined reactor. The reactor was kept at 433 K for 120 h under autogenous pressure. Single crystals of the title compound were obtained after cooling to room temperature.
H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.93Å and O—H = 0.82 Å, and with Uiso(H) = 1.2Ueq(C) and Uiso(H) = 1.5Ueq(O).
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Siemens, 1990); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
[Co(C16H8O8)(C10H8N2)2] | Z = 2 |
Mr = 699.52 | F(000) = 718 |
Triclinic, P1 | Dx = 1.561 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 11.045 (2) Å | Cell parameters from 14754 reflections |
b = 11.361 (2) Å | θ = 3.2–27.5° |
c = 12.352 (3) Å | µ = 0.64 mm−1 |
α = 103.83 (3)° | T = 298 K |
β = 93.54 (3)° | Block, purple |
γ = 96.84 (3)° | 0.24 × 0.22 × 0.17 mm |
V = 1487.8 (6) Å3 |
Bruker SMART APEX CCD area-detector diffractometer | 6747 independent reflections |
Radiation source: fine-focus sealed tube | 5292 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
ϕ and ω scans | θmax = 27.5°, θmin = 3.2° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −14→14 |
Tmin = 0.856, Tmax = 0.898 | k = −14→14 |
14754 measured reflections | l = −16→16 |
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) = 0.123 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0823P)2 + 0.1308P] where P = (Fo2 + 2Fc2)/3 |
6747 reflections | (Δ/σ)max = 0.003 |
442 parameters | Δρmax = 0.42 e Å−3 |
0 restraints | Δρmin = −0.32 e Å−3 |
[Co(C16H8O8)(C10H8N2)2] | γ = 96.84 (3)° |
Mr = 699.52 | V = 1487.8 (6) Å3 |
Triclinic, P1 | Z = 2 |
a = 11.045 (2) Å | Mo Kα radiation |
b = 11.361 (2) Å | µ = 0.64 mm−1 |
c = 12.352 (3) Å | T = 298 K |
α = 103.83 (3)° | 0.24 × 0.22 × 0.17 mm |
β = 93.54 (3)° |
Bruker SMART APEX CCD area-detector diffractometer | 6747 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 5292 reflections with I > 2σ(I) |
Tmin = 0.856, Tmax = 0.898 | Rint = 0.025 |
14754 measured reflections |
R[F2 > 2σ(F2)] = 0.041 | 0 restraints |
wR(F2) = 0.123 | H-atom parameters constrained |
S = 1.01 | Δρmax = 0.42 e Å−3 |
6747 reflections | Δρmin = −0.32 e Å−3 |
442 parameters |
x | y | z | Uiso*/Ueq | ||
Co1 | 0.15335 (3) | 0.02558 (3) | 0.13743 (2) | 0.02485 (10) | |
C1 | −0.2712 (2) | −0.4174 (2) | 0.4984 (2) | 0.0394 (6) | |
H1A | −0.2746 | −0.4011 | 0.5755 | 0.047* | |
C2 | −0.1971 (2) | −0.3366 (2) | 0.4554 (2) | 0.0358 (5) | |
H2A | −0.1517 | −0.2675 | 0.5033 | 0.043* | |
C3 | −0.1905 (2) | −0.3584 (2) | 0.34135 (19) | 0.0305 (5) | |
C4 | −0.2601 (3) | −0.4642 (2) | 0.2740 (2) | 0.0408 (6) | |
H4A | −0.2581 | −0.4832 | 0.1967 | 0.049* | |
C5 | −0.3324 (3) | −0.5404 (2) | 0.3241 (2) | 0.0445 (6) | |
H5A | −0.3789 | −0.6104 | 0.2786 | 0.053* | |
C6 | −0.0178 (2) | −0.0684 (2) | 0.2993 (2) | 0.0326 (5) | |
H6A | 0.0000 | 0.0132 | 0.3387 | 0.039* | |
C7 | −0.0854 (2) | −0.1485 (2) | 0.3482 (2) | 0.0343 (5) | |
H7A | −0.1114 | −0.1206 | 0.4189 | 0.041* | |
C8 | −0.1146 (2) | −0.2714 (2) | 0.29093 (19) | 0.0300 (5) | |
C9 | −0.0714 (3) | −0.3060 (2) | 0.1874 (2) | 0.0411 (6) | |
H9A | −0.0875 | −0.3872 | 0.1464 | 0.049* | |
C10 | −0.0039 (2) | −0.2195 (2) | 0.1442 (2) | 0.0379 (6) | |
H10A | 0.0236 | −0.2450 | 0.0738 | 0.046* | |
C11 | 0.4115 (2) | 0.1192 (3) | 0.0882 (2) | 0.0438 (6) | |
H11A | 0.4308 | 0.0591 | 0.1234 | 0.053* | |
C12 | 0.5048 (2) | 0.1784 (3) | 0.0424 (2) | 0.0445 (6) | |
H12A | 0.5838 | 0.1583 | 0.0471 | 0.053* | |
C13 | 0.4781 (2) | 0.2676 (2) | −0.0102 (2) | 0.0361 (5) | |
C14 | 0.3604 (3) | 0.2964 (3) | −0.0087 (3) | 0.0567 (9) | |
H14A | 0.3396 | 0.3588 | −0.0401 | 0.068* | |
C15 | 0.2728 (3) | 0.2327 (3) | 0.0393 (3) | 0.0510 (7) | |
H15A | 0.1941 | 0.2540 | 0.0393 | 0.061* | |
C16 | 0.7799 (3) | 0.4056 (3) | −0.0840 (3) | 0.0499 (7) | |
H16A | 0.8623 | 0.4185 | −0.0576 | 0.060* | |
C17 | 0.6967 (3) | 0.3472 (3) | −0.0289 (3) | 0.0459 (6) | |
H17A | 0.7230 | 0.3194 | 0.0323 | 0.055* | |
C18 | 0.5733 (2) | 0.3304 (2) | −0.0655 (2) | 0.0366 (5) | |
C19 | 0.5395 (3) | 0.3744 (3) | −0.1559 (2) | 0.0524 (8) | |
H19A | 0.4574 | 0.3664 | −0.1818 | 0.063* | |
C20 | 0.6290 (3) | 0.4308 (3) | −0.2083 (3) | 0.0584 (9) | |
H20A | 0.6051 | 0.4600 | −0.2694 | 0.070* | |
C21 | 0.22465 (19) | −0.14137 (19) | 0.63711 (17) | 0.0251 (4) | |
C22 | 0.20320 (19) | −0.10850 (19) | 0.74957 (17) | 0.0252 (4) | |
H22A | 0.2433 | −0.0351 | 0.7951 | 0.030* | |
C23 | 0.12327 (19) | −0.18306 (19) | 0.79495 (17) | 0.0240 (4) | |
C24 | 0.0677 (2) | −0.29749 (19) | 0.72797 (17) | 0.0260 (4) | |
C25 | 0.0908 (2) | −0.3316 (2) | 0.61661 (19) | 0.0314 (5) | |
H25A | 0.0546 | −0.4070 | 0.5719 | 0.038* | |
C26 | 0.1675 (2) | −0.2542 (2) | 0.57121 (18) | 0.0298 (5) | |
H26A | 0.1810 | −0.2777 | 0.4960 | 0.036* | |
C27 | 0.29693 (19) | −0.05148 (19) | 0.58818 (17) | 0.0255 (4) | |
C28 | 0.3919 (2) | 0.0341 (2) | 0.65183 (18) | 0.0303 (5) | |
H28A | 0.4156 | 0.0310 | 0.7246 | 0.036* | |
C29 | 0.4510 (2) | 0.1239 (2) | 0.60680 (19) | 0.0304 (5) | |
H29A | 0.5150 | 0.1795 | 0.6494 | 0.036* | |
C30 | 0.41605 (19) | 0.13164 (19) | 0.49935 (18) | 0.0261 (4) | |
C31 | 0.32276 (19) | 0.04471 (19) | 0.43401 (17) | 0.0266 (4) | |
C32 | 0.26553 (19) | −0.04591 (19) | 0.47919 (18) | 0.0269 (4) | |
H32A | 0.2046 | −0.1043 | 0.4352 | 0.032* | |
C33 | 0.08564 (19) | −0.13041 (17) | 0.90973 (17) | 0.0242 (4) | |
C34 | −0.0092 (2) | −0.3814 (2) | 0.78063 (19) | 0.0312 (5) | |
C35 | 0.4801 (2) | 0.2274 (2) | 0.4504 (2) | 0.0319 (5) | |
C36 | 0.2723 (2) | 0.0462 (2) | 0.31868 (17) | 0.0281 (5) | |
N1 | −0.3384 (2) | −0.51818 (19) | 0.43373 (19) | 0.0401 (5) | |
N2 | 0.02360 (18) | −0.10141 (17) | 0.19870 (16) | 0.0293 (4) | |
N3 | 0.29647 (18) | 0.14250 (18) | 0.08518 (16) | 0.0330 (4) | |
N4 | 0.7468 (2) | 0.4445 (2) | −0.1744 (2) | 0.0491 (6) | |
O1 | 0.16807 (14) | −0.09749 (14) | 0.98893 (12) | 0.0299 (3) | |
O2 | −0.02537 (14) | −0.11935 (13) | 0.91601 (13) | 0.0291 (3) | |
O3 | 0.01081 (18) | −0.38419 (15) | 0.87748 (14) | 0.0411 (4) | |
O4 | −0.09660 (19) | −0.45426 (19) | 0.71183 (16) | 0.0562 (6) | |
H1 | −0.1328 | −0.5005 | 0.7447 | 0.084* | |
O5 | 0.54844 (18) | 0.31614 (16) | 0.52605 (15) | 0.0448 (5) | |
H2 | 0.5974 | 0.3535 | 0.4947 | 0.067* | |
O6 | 0.47072 (19) | 0.22331 (17) | 0.35211 (15) | 0.0484 (5) | |
O7 | 0.29338 (16) | −0.03486 (15) | 0.23673 (13) | 0.0345 (4) | |
O8 | 0.19877 (15) | 0.12079 (14) | 0.30946 (13) | 0.0327 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.02672 (17) | 0.02842 (16) | 0.02075 (16) | −0.00082 (11) | 0.00528 (11) | 0.01020 (11) |
C1 | 0.0426 (14) | 0.0436 (13) | 0.0367 (13) | 0.0014 (11) | 0.0108 (11) | 0.0192 (11) |
C2 | 0.0367 (13) | 0.0370 (12) | 0.0343 (13) | −0.0013 (10) | 0.0073 (10) | 0.0124 (10) |
C3 | 0.0327 (11) | 0.0293 (10) | 0.0341 (12) | 0.0032 (9) | 0.0097 (9) | 0.0157 (9) |
C4 | 0.0504 (15) | 0.0369 (12) | 0.0357 (13) | −0.0034 (11) | 0.0053 (11) | 0.0141 (10) |
C5 | 0.0497 (15) | 0.0352 (12) | 0.0474 (15) | −0.0095 (12) | 0.0016 (12) | 0.0163 (11) |
C6 | 0.0327 (12) | 0.0288 (10) | 0.0372 (13) | 0.0004 (9) | 0.0109 (10) | 0.0101 (9) |
C7 | 0.0380 (13) | 0.0335 (11) | 0.0332 (12) | 0.0026 (10) | 0.0136 (10) | 0.0106 (9) |
C8 | 0.0313 (11) | 0.0304 (10) | 0.0330 (12) | 0.0016 (9) | 0.0092 (9) | 0.0168 (9) |
C9 | 0.0610 (17) | 0.0260 (11) | 0.0366 (13) | −0.0023 (11) | 0.0161 (12) | 0.0098 (9) |
C10 | 0.0507 (15) | 0.0342 (12) | 0.0304 (12) | −0.0006 (11) | 0.0156 (11) | 0.0111 (9) |
C11 | 0.0404 (14) | 0.0503 (15) | 0.0523 (16) | 0.0076 (12) | 0.0156 (12) | 0.0316 (13) |
C12 | 0.0333 (13) | 0.0543 (15) | 0.0556 (17) | 0.0072 (11) | 0.0162 (12) | 0.0289 (13) |
C13 | 0.0330 (12) | 0.0383 (12) | 0.0387 (13) | −0.0034 (10) | 0.0114 (10) | 0.0151 (10) |
C14 | 0.0394 (15) | 0.0617 (18) | 0.089 (2) | 0.0074 (14) | 0.0188 (15) | 0.0543 (18) |
C15 | 0.0317 (13) | 0.0573 (17) | 0.078 (2) | 0.0061 (12) | 0.0166 (13) | 0.0419 (16) |
C16 | 0.0380 (14) | 0.0544 (16) | 0.0610 (18) | −0.0032 (13) | 0.0138 (13) | 0.0238 (14) |
C17 | 0.0388 (14) | 0.0515 (15) | 0.0553 (17) | 0.0042 (12) | 0.0144 (12) | 0.0267 (13) |
C18 | 0.0359 (13) | 0.0353 (12) | 0.0392 (13) | −0.0051 (10) | 0.0104 (10) | 0.0137 (10) |
C19 | 0.0391 (14) | 0.0689 (18) | 0.0499 (17) | −0.0149 (14) | 0.0027 (12) | 0.0274 (15) |
C20 | 0.0585 (19) | 0.075 (2) | 0.0430 (16) | −0.0173 (16) | 0.0041 (14) | 0.0294 (15) |
C21 | 0.0247 (10) | 0.0301 (10) | 0.0243 (10) | 0.0007 (8) | 0.0081 (8) | 0.0141 (8) |
C22 | 0.0261 (10) | 0.0278 (10) | 0.0218 (10) | −0.0016 (8) | 0.0055 (8) | 0.0081 (8) |
C23 | 0.0238 (10) | 0.0301 (10) | 0.0206 (10) | 0.0009 (8) | 0.0053 (8) | 0.0116 (8) |
C24 | 0.0272 (10) | 0.0268 (10) | 0.0247 (10) | −0.0029 (8) | 0.0059 (8) | 0.0103 (8) |
C25 | 0.0359 (12) | 0.0273 (10) | 0.0279 (11) | −0.0058 (9) | 0.0064 (9) | 0.0050 (8) |
C26 | 0.0348 (12) | 0.0334 (11) | 0.0214 (10) | −0.0007 (9) | 0.0085 (9) | 0.0082 (8) |
C27 | 0.0253 (10) | 0.0299 (10) | 0.0240 (10) | −0.0001 (8) | 0.0099 (8) | 0.0119 (8) |
C28 | 0.0306 (11) | 0.0393 (12) | 0.0224 (10) | −0.0016 (9) | 0.0043 (9) | 0.0133 (9) |
C29 | 0.0291 (11) | 0.0323 (11) | 0.0286 (11) | −0.0067 (9) | 0.0027 (9) | 0.0109 (9) |
C30 | 0.0251 (10) | 0.0289 (10) | 0.0263 (10) | −0.0013 (8) | 0.0069 (8) | 0.0119 (8) |
C31 | 0.0261 (10) | 0.0312 (10) | 0.0243 (10) | −0.0011 (9) | 0.0076 (8) | 0.0118 (8) |
C32 | 0.0251 (10) | 0.0318 (10) | 0.0247 (10) | −0.0035 (8) | 0.0056 (8) | 0.0115 (8) |
C33 | 0.0298 (11) | 0.0209 (9) | 0.0249 (10) | −0.0001 (8) | 0.0100 (8) | 0.0109 (8) |
C34 | 0.0342 (12) | 0.0288 (10) | 0.0312 (12) | −0.0026 (9) | 0.0093 (9) | 0.0103 (9) |
C35 | 0.0285 (11) | 0.0344 (11) | 0.0349 (12) | −0.0033 (9) | 0.0074 (9) | 0.0155 (9) |
C36 | 0.0278 (11) | 0.0338 (11) | 0.0232 (10) | −0.0081 (9) | 0.0044 (8) | 0.0136 (9) |
N1 | 0.0394 (12) | 0.0381 (11) | 0.0468 (13) | −0.0028 (9) | 0.0088 (9) | 0.0215 (9) |
N2 | 0.0314 (10) | 0.0299 (9) | 0.0291 (10) | 0.0013 (8) | 0.0056 (8) | 0.0130 (7) |
N3 | 0.0318 (10) | 0.0367 (10) | 0.0327 (10) | −0.0005 (8) | 0.0078 (8) | 0.0143 (8) |
N4 | 0.0441 (13) | 0.0528 (13) | 0.0494 (14) | −0.0132 (11) | 0.0161 (11) | 0.0174 (11) |
O1 | 0.0298 (8) | 0.0388 (8) | 0.0208 (7) | 0.0028 (6) | 0.0047 (6) | 0.0070 (6) |
O2 | 0.0276 (8) | 0.0310 (8) | 0.0322 (8) | 0.0037 (6) | 0.0097 (6) | 0.0134 (6) |
O3 | 0.0549 (11) | 0.0380 (9) | 0.0319 (9) | −0.0068 (8) | 0.0074 (8) | 0.0173 (7) |
O4 | 0.0526 (12) | 0.0673 (13) | 0.0427 (11) | −0.0335 (10) | −0.0005 (9) | 0.0235 (10) |
O5 | 0.0527 (11) | 0.0393 (9) | 0.0391 (10) | −0.0201 (8) | 0.0045 (8) | 0.0162 (8) |
O6 | 0.0568 (12) | 0.0530 (11) | 0.0345 (10) | −0.0184 (9) | 0.0026 (8) | 0.0222 (8) |
O7 | 0.0388 (9) | 0.0409 (9) | 0.0245 (8) | 0.0020 (7) | 0.0055 (7) | 0.0107 (7) |
O8 | 0.0385 (9) | 0.0331 (8) | 0.0275 (8) | 0.0018 (7) | 0.0024 (7) | 0.0108 (6) |
Co1—O2i | 2.0369 (16) | C17—C18 | 1.385 (4) |
Co1—O1ii | 2.0519 (17) | C17—H17A | 0.9300 |
Co1—O8 | 2.1394 (18) | C18—C19 | 1.376 (4) |
Co1—N3 | 2.1716 (19) | C19—C20 | 1.391 (4) |
Co1—O7 | 2.1885 (18) | C19—H19A | 0.9300 |
Co1—N2 | 2.2072 (19) | C20—N4 | 1.321 (4) |
Co1—C36 | 2.471 (2) | C20—H20A | 0.9300 |
C1—N1 | 1.337 (3) | C21—C22 | 1.392 (3) |
C1—C2 | 1.378 (3) | C21—C26 | 1.396 (3) |
C1—H1A | 0.9300 | C21—C27 | 1.485 (3) |
C2—C3 | 1.380 (3) | C22—C23 | 1.386 (3) |
C2—H2A | 0.9300 | C22—H22A | 0.9300 |
C3—C4 | 1.397 (3) | C23—C24 | 1.408 (3) |
C3—C8 | 1.494 (3) | C23—C33 | 1.506 (3) |
C4—C5 | 1.387 (3) | C24—C25 | 1.385 (3) |
C4—H4A | 0.9300 | C24—C34 | 1.492 (3) |
C5—N1 | 1.324 (3) | C25—C26 | 1.386 (3) |
C5—H5A | 0.9300 | C25—H25A | 0.9300 |
C6—N2 | 1.335 (3) | C26—H26A | 0.9300 |
C6—C7 | 1.381 (3) | C27—C32 | 1.387 (3) |
C6—H6A | 0.9300 | C27—C28 | 1.397 (3) |
C7—C8 | 1.395 (3) | C28—C29 | 1.391 (3) |
C7—H7A | 0.9300 | C28—H28A | 0.9300 |
C8—C9 | 1.377 (3) | C29—C30 | 1.385 (3) |
C9—C10 | 1.390 (3) | C29—H29A | 0.9300 |
C9—H9A | 0.9300 | C30—C31 | 1.401 (3) |
C10—N2 | 1.339 (3) | C30—C35 | 1.494 (3) |
C10—H10A | 0.9300 | C31—C32 | 1.391 (3) |
C11—N3 | 1.329 (3) | C31—C36 | 1.502 (3) |
C11—C12 | 1.386 (3) | C32—H32A | 0.9300 |
C11—H11A | 0.9300 | C33—O1 | 1.249 (3) |
C12—C13 | 1.378 (3) | C33—O2 | 1.253 (3) |
C12—H12A | 0.9300 | C34—O3 | 1.212 (3) |
C13—C14 | 1.378 (4) | C34—O4 | 1.308 (3) |
C13—C18 | 1.492 (3) | C35—O6 | 1.201 (3) |
C14—C15 | 1.386 (4) | C35—O5 | 1.319 (3) |
C14—H14A | 0.9300 | C36—O7 | 1.250 (3) |
C15—N3 | 1.328 (3) | C36—O8 | 1.261 (3) |
C15—H15A | 0.9300 | O1—Co1iii | 2.0519 (17) |
C16—N4 | 1.342 (4) | O2—Co1i | 2.0369 (16) |
C16—C17 | 1.378 (3) | O4—H1 | 0.8200 |
C16—H16A | 0.9300 | O5—H2 | 0.8200 |
O2i—Co1—O1ii | 99.25 (7) | C19—C18—C13 | 119.9 (2) |
O2i—Co1—O8 | 103.34 (7) | C17—C18—C13 | 122.2 (2) |
O1ii—Co1—O8 | 157.16 (7) | C18—C19—C20 | 119.6 (3) |
O2i—Co1—N3 | 89.85 (7) | C18—C19—H19A | 120.2 |
O1ii—Co1—N3 | 85.19 (7) | C20—C19—H19A | 120.2 |
O8—Co1—N3 | 91.48 (7) | N4—C20—C19 | 122.4 (3) |
O2i—Co1—O7 | 164.24 (6) | N4—C20—H20A | 118.8 |
O1ii—Co1—O7 | 96.34 (7) | C19—C20—H20A | 118.8 |
O8—Co1—O7 | 60.97 (7) | C22—C21—C26 | 118.49 (18) |
N3—Co1—O7 | 89.13 (7) | C22—C21—C27 | 119.44 (19) |
O2i—Co1—N2 | 96.19 (7) | C26—C21—C27 | 121.79 (19) |
O1ii—Co1—N2 | 94.62 (7) | C23—C22—C21 | 121.28 (19) |
O8—Co1—N2 | 86.34 (7) | C23—C22—H22A | 119.4 |
N3—Co1—N2 | 173.91 (7) | C21—C22—H22A | 119.4 |
O7—Co1—N2 | 84.84 (7) | C22—C23—C24 | 119.57 (19) |
O2i—Co1—C36 | 134.01 (8) | C22—C23—C33 | 117.84 (18) |
O1ii—Co1—C36 | 126.68 (8) | C24—C23—C33 | 122.03 (17) |
O8—Co1—C36 | 30.67 (7) | C25—C24—C23 | 119.23 (18) |
N3—Co1—C36 | 91.59 (7) | C25—C24—C34 | 121.77 (19) |
O7—Co1—C36 | 30.34 (7) | C23—C24—C34 | 118.92 (19) |
N2—Co1—C36 | 83.63 (7) | C24—C25—C26 | 120.6 (2) |
N1—C1—C2 | 122.7 (2) | C24—C25—H25A | 119.7 |
N1—C1—H1A | 118.6 | C26—C25—H25A | 119.7 |
C2—C1—H1A | 118.6 | C25—C26—C21 | 120.8 (2) |
C3—C2—C1 | 119.9 (2) | C25—C26—H26A | 119.6 |
C3—C2—H2A | 120.1 | C21—C26—H26A | 119.6 |
C1—C2—H2A | 120.1 | C32—C27—C28 | 118.43 (18) |
C2—C3—C4 | 117.3 (2) | C32—C27—C21 | 119.95 (19) |
C2—C3—C8 | 121.7 (2) | C28—C27—C21 | 121.48 (18) |
C4—C3—C8 | 121.0 (2) | C29—C28—C27 | 120.23 (19) |
C5—C4—C3 | 119.0 (2) | C29—C28—H28A | 119.9 |
C5—C4—H4A | 120.5 | C27—C28—H28A | 119.9 |
C3—C4—H4A | 120.5 | C30—C29—C28 | 121.0 (2) |
N1—C5—C4 | 123.1 (2) | C30—C29—H29A | 119.5 |
N1—C5—H5A | 118.5 | C28—C29—H29A | 119.5 |
C4—C5—H5A | 118.5 | C29—C30—C31 | 119.22 (18) |
N2—C6—C7 | 123.8 (2) | C29—C30—C35 | 121.1 (2) |
N2—C6—H6A | 118.1 | C31—C30—C35 | 119.62 (19) |
C7—C6—H6A | 118.1 | C32—C31—C30 | 119.32 (19) |
C6—C7—C8 | 119.6 (2) | C32—C31—C36 | 116.05 (18) |
C6—C7—H7A | 120.2 | C30—C31—C36 | 124.49 (17) |
C8—C7—H7A | 120.2 | C27—C32—C31 | 121.76 (19) |
C9—C8—C7 | 116.82 (19) | C27—C32—H32A | 119.1 |
C9—C8—C3 | 122.9 (2) | C31—C32—H32A | 119.1 |
C7—C8—C3 | 120.2 (2) | O1—C33—O2 | 126.0 (2) |
C8—C9—C10 | 119.9 (2) | O1—C33—C23 | 117.37 (19) |
C8—C9—H9A | 120.0 | O2—C33—C23 | 116.58 (19) |
C10—C9—H9A | 120.0 | O3—C34—O4 | 123.4 (2) |
N2—C10—C9 | 123.3 (2) | O3—C34—C24 | 122.6 (2) |
N2—C10—H10A | 118.3 | O4—C34—C24 | 113.95 (19) |
C9—C10—H10A | 118.3 | O6—C35—O5 | 123.6 (2) |
N3—C11—C12 | 124.4 (2) | O6—C35—C30 | 123.3 (2) |
N3—C11—H11A | 117.8 | O5—C35—C30 | 113.08 (19) |
C12—C11—H11A | 117.8 | O7—C36—O8 | 122.0 (2) |
C13—C12—C11 | 118.7 (2) | O7—C36—C31 | 119.0 (2) |
C13—C12—H12A | 120.6 | O8—C36—C31 | 118.4 (2) |
C11—C12—H12A | 120.6 | O7—C36—Co1 | 62.22 (12) |
C14—C13—C12 | 117.2 (2) | O8—C36—Co1 | 59.96 (11) |
C14—C13—C18 | 121.8 (2) | C31—C36—Co1 | 168.81 (14) |
C12—C13—C18 | 121.1 (2) | C5—N1—C1 | 117.9 (2) |
C13—C14—C15 | 120.2 (2) | C6—N2—C10 | 116.49 (19) |
C13—C14—H14A | 119.9 | C6—N2—Co1 | 121.34 (15) |
C15—C14—H14A | 119.9 | C10—N2—Co1 | 121.53 (16) |
N3—C15—C14 | 122.8 (3) | C15—N3—C11 | 116.5 (2) |
N3—C15—H15A | 118.6 | C15—N3—Co1 | 122.41 (17) |
C14—C15—H15A | 118.6 | C11—N3—Co1 | 120.75 (16) |
N4—C16—C17 | 122.6 (3) | C20—N4—C16 | 118.2 (2) |
N4—C16—H16A | 118.7 | C33—O1—Co1iii | 124.20 (15) |
C17—C16—H16A | 118.7 | C33—O2—Co1i | 139.83 (13) |
C16—C17—C18 | 119.3 (3) | C34—O4—H1 | 109.2 |
C16—C17—H17A | 120.4 | C35—O5—H2 | 109.2 |
C18—C17—H17A | 120.4 | C36—O7—Co1 | 87.44 (14) |
C19—C18—C17 | 117.8 (2) | C36—O8—Co1 | 89.37 (13) |
Symmetry codes: (i) −x, −y, −z+1; (ii) x, y, z−1; (iii) x, y, z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H1···N4iv | 0.82 | 1.85 | 2.624 (3) | 157 |
O5—H2···N1v | 0.82 | 1.88 | 2.655 (2) | 157 |
Symmetry codes: (iv) x−1, y−1, z+1; (v) x+1, y+1, z. |
Experimental details
Crystal data | |
Chemical formula | [Co(C16H8O8)(C10H8N2)2] |
Mr | 699.52 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 298 |
a, b, c (Å) | 11.045 (2), 11.361 (2), 12.352 (3) |
α, β, γ (°) | 103.83 (3), 93.54 (3), 96.84 (3) |
V (Å3) | 1487.8 (6) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.64 |
Crystal size (mm) | 0.24 × 0.22 × 0.17 |
Data collection | |
Diffractometer | Bruker SMART APEX CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.856, 0.898 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14754, 6747, 5292 |
Rint | 0.025 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.123, 1.01 |
No. of reflections | 6747 |
No. of parameters | 442 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.42, −0.32 |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Siemens, 1990).
Co1—O2i | 2.0369 (16) | Co1—N3 | 2.1716 (19) |
Co1—O1ii | 2.0519 (17) | Co1—O7 | 2.1885 (18) |
Co1—O8 | 2.1394 (18) | Co1—N2 | 2.2072 (19) |
O2i—Co1—O1ii | 99.25 (7) | O8—Co1—O7 | 60.97 (7) |
O2i—Co1—O8 | 103.34 (7) | N3—Co1—O7 | 89.13 (7) |
O1ii—Co1—O8 | 157.16 (7) | O2i—Co1—N2 | 96.19 (7) |
O2i—Co1—N3 | 89.85 (7) | O1ii—Co1—N2 | 94.62 (7) |
O1ii—Co1—N3 | 85.19 (7) | O8—Co1—N2 | 86.34 (7) |
O8—Co1—N3 | 91.48 (7) | N3—Co1—N2 | 173.91 (7) |
O2i—Co1—O7 | 164.24 (6) | O7—Co1—N2 | 84.84 (7) |
O1ii—Co1—O7 | 96.34 (7) |
Symmetry codes: (i) −x, −y, −z+1; (ii) x, y, z−1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H1···N4iii | 0.82 | 1.85 | 2.624 (3) | 157 |
O5—H2···N1iv | 0.82 | 1.88 | 2.655 (2) | 157 |
Symmetry codes: (iii) x−1, y−1, z+1; (iv) x+1, y+1, z. |
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Metal–carboxylate coordination polymers have emerged as an important family in the past few years (Wang et al., 2005; Hao et al., 2005). We report here the structure of the title compound. The asymmetric unit contains one CoII atom, one 4,4'-dicarboxybiphenyl-3,3'-dicarboxylate (bpdc) ligand and two 4,4'-bipyridine (4,4'-bpy) ligands. The CoII atom has a distorted octahedral coordination geometry, defined by four O atoms from the bpdc ligands and two N atoms from the 4,4'-bpy ligands. The adjacent CoII atoms are linked by the bpdc ligands to generate a one-dimensional chain running along the crystallographic c axis. In the crystal structure, the adjacent one-dimensional chains are further connected with O—H···N hydrogen bonds, forming a two-dimensional supramolecular network.