Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807057959/ng2367sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807057959/ng2367Isup2.hkl |
CCDC reference: 672680
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.005 Å
- R factor = 0.043
- wR factor = 0.142
- Data-to-parameter ratio = 15.9
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 105.00 A 3
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 3000 Deg. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Co1 (9) 1.28 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 6
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 2 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 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For the 1,10-phenanthroline-coordinated nickel derivative of trans-stilbene-4,4'-dicarboxylic acid, see Wang, Gao et al. (2006). For other zinc and cadmium complexes, see Wang et al. (2004); Wang, Qin et al. (2006). [Please note that the Related literature section must contain all those references, and only those references, that are cited in the Supplementary material. It cannot be used to cite references that are not cited elsewhere in the CIF. Thus, Wang, Gao et al. (2006) will be removed, unless you wish to provide a revised Comment or other section which cites it.]
A mixture of CoCl2.6H2O (1 mmol), 1,10-phenanthroline (1 mmol), trans-stilbene-4,4'-dicarboxylic acid(1 mmol) and water (10 ml) was stirred for 15 min in air, then transferred and sealed in a 23 ml Parr teflon-lined stainless steel vessel, heated to 160 ° for 5 days, and then cooled to room temperature. The resulting red crystals were filtered, washed, and dried in air. Analysis calculated for C28H22CoN2O6: C 62.12, H 4.10, N 5.17%; found: C 62.14, H 4.13, N 5.15%.
The H atoms were placed in calculated positions with C—H = 0.93 or 0.97 Å and Uiso(H) = 1.2Ueq(C) and were included in the refinement in the riding model approximation. The H atoms of hydroxyl groups were located in difference Fourier maps and refined with the O—H distance restrained to 0.85 (1) Å and Uiso(H) = 1.5Ueq(O).
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: publCIF (Westrip 2007).
Fig. 1. Molecular structure of the title compound. Dashed lines indicate O—H···O hydrogen bonds. | |
Fig. 2. The packing diagram of the title complex, with the hydrogen bonds denoted by dashed lines. |
[Co(C16H10O4)(C12H8N2)H2O)2] | Z = 2 |
Mr = 541.41 | F(000) = 558 |
Triclinic, P1 | Dx = 1.446 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.5345 (15) Å | Cell parameters from 10169 reflections |
b = 9.2112 (18) Å | θ = 3.1–27.5° |
c = 18.524 (4) Å | µ = 0.74 mm−1 |
α = 88.12 (3)° | T = 295 K |
β = 84.29 (3)° | Prism, pink |
γ = 76.38 (3)° | 0.36 × 0.24 × 0.12 mm |
V = 1243.2 (5) Å3 |
Rigaku R-AXIS RAPID diffractometer | 5509 independent reflections |
Radiation source: fine-focus sealed tube | 4338 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
Detector resolution: 10 pixels mm-1 | θmax = 27.5°, θmin = 3.1° |
ω scans | h = −9→9 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −11→11 |
Tmin = 0.811, Tmax = 0.917 | l = −23→24 |
11895 measured reflections |
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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.142 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0745P)2 + 1.1034P] where P = (Fo2 + 2Fc2)/3 |
5509 reflections | (Δ/σ)max < 0.001 |
346 parameters | Δρmax = 0.47 e Å−3 |
6 restraints | Δρmin = −0.48 e Å−3 |
[Co(C16H10O4)(C12H8N2)H2O)2] | γ = 76.38 (3)° |
Mr = 541.41 | V = 1243.2 (5) Å3 |
Triclinic, P1 | Z = 2 |
a = 7.5345 (15) Å | Mo Kα radiation |
b = 9.2112 (18) Å | µ = 0.74 mm−1 |
c = 18.524 (4) Å | T = 295 K |
α = 88.12 (3)° | 0.36 × 0.24 × 0.12 mm |
β = 84.29 (3)° |
Rigaku R-AXIS RAPID diffractometer | 5509 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 4338 reflections with I > 2σ(I) |
Tmin = 0.811, Tmax = 0.917 | Rint = 0.030 |
11895 measured reflections |
R[F2 > 2σ(F2)] = 0.043 | 6 restraints |
wR(F2) = 0.142 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | Δρmax = 0.47 e Å−3 |
5509 reflections | Δρmin = −0.48 e Å−3 |
346 parameters |
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 | 0.43923 (5) | 0.65500 (4) | 0.628861 (19) | 0.02933 (13) | |
O1W | 0.6521 (3) | 0.5294 (3) | 0.55787 (12) | 0.0440 (5) | |
H1W1 | 0.675 (5) | 0.513 (5) | 0.5126 (7) | 0.066* | |
H1W2 | 0.744 (3) | 0.549 (5) | 0.5747 (17) | 0.066* | |
O2W | 0.2624 (3) | 0.5328 (2) | 0.58733 (10) | 0.0347 (4) | |
H2W1 | 0.1490 (17) | 0.559 (3) | 0.6021 (18) | 0.052* | |
H2W2 | 0.310 (4) | 0.451 (2) | 0.6084 (18) | 0.052* | |
O1 | 0.3931 (3) | 0.3052 (2) | 0.66551 (12) | 0.0458 (5) | |
O2 | 0.4849 (3) | 0.4951 (2) | 0.71028 (11) | 0.0428 (5) | |
O3 | 0.9059 (3) | 0.5857 (3) | 0.63524 (11) | 0.0441 (5) | |
O4 | 0.6409 (3) | 0.7378 (2) | 0.67405 (11) | 0.0347 (4) | |
N1 | 0.2421 (3) | 0.8101 (3) | 0.69611 (13) | 0.0368 (5) | |
N2 | 0.3447 (3) | 0.8322 (3) | 0.55504 (13) | 0.0339 (5) | |
C1 | 0.1957 (5) | 0.7976 (4) | 0.76617 (18) | 0.0500 (8) | |
H1A | 0.2489 | 0.7107 | 0.7904 | 0.060* | |
C2 | 0.0693 (6) | 0.9103 (5) | 0.8053 (2) | 0.0656 (12) | |
H2A | 0.0391 | 0.8979 | 0.8547 | 0.079* | |
C3 | −0.0089 (6) | 1.0383 (5) | 0.7706 (3) | 0.0683 (12) | |
H3A | −0.0946 | 1.1129 | 0.7961 | 0.082* | |
C4 | 0.0386 (5) | 1.0581 (4) | 0.6969 (2) | 0.0524 (9) | |
C5 | −0.0311 (5) | 1.1907 (4) | 0.6553 (3) | 0.0650 (12) | |
H5A | −0.1155 | 1.2703 | 0.6779 | 0.078* | |
C6 | 0.0238 (5) | 1.2009 (4) | 0.5847 (3) | 0.0612 (11) | |
H6A | −0.0231 | 1.2882 | 0.5594 | 0.073* | |
C7 | 0.1512 (4) | 1.0830 (3) | 0.5473 (2) | 0.0452 (8) | |
C8 | 0.2095 (5) | 1.0866 (4) | 0.4735 (2) | 0.0523 (9) | |
H8A | 0.1656 | 1.1712 | 0.4459 | 0.063* | |
C9 | 0.3301 (5) | 0.9673 (4) | 0.44203 (19) | 0.0486 (8) | |
H9A | 0.3696 | 0.9696 | 0.3929 | 0.058* | |
C10 | 0.3943 (5) | 0.8406 (4) | 0.48433 (16) | 0.0417 (7) | |
H10A | 0.4752 | 0.7587 | 0.4620 | 0.050* | |
C11 | 0.2226 (4) | 0.9508 (3) | 0.58613 (17) | 0.0354 (6) | |
C12 | 0.1659 (4) | 0.9390 (3) | 0.66163 (17) | 0.0378 (7) | |
C13 | 0.7921 (4) | 0.6514 (3) | 0.68497 (15) | 0.0314 (6) | |
C14 | 0.8366 (4) | 0.6222 (3) | 0.76200 (15) | 0.0348 (6) | |
C15 | 0.7248 (5) | 0.7048 (4) | 0.81696 (18) | 0.0522 (9) | |
H15A | 0.6250 | 0.7798 | 0.8056 | 0.063* | |
C16 | 0.7589 (6) | 0.6776 (5) | 0.88847 (19) | 0.0627 (11) | |
H16A | 0.6814 | 0.7347 | 0.9245 | 0.075* | |
C17 | 0.9054 (5) | 0.5675 (5) | 0.90771 (18) | 0.0539 (9) | |
C18 | 1.0162 (5) | 0.4823 (4) | 0.85223 (19) | 0.0515 (9) | |
H18A | 1.1141 | 0.4057 | 0.8638 | 0.062* | |
C19 | 0.9832 (4) | 0.5096 (4) | 0.78023 (17) | 0.0416 (7) | |
H19A | 1.0596 | 0.4522 | 0.7440 | 0.050* | |
C20 | 0.9339 (6) | 0.5462 (5) | 0.9859 (2) | 0.0654 (11) | |
H20A | 0.8468 | 0.6061 | 1.0181 | 0.079* | |
C21 | 0.4532 (4) | 0.3663 (3) | 0.71367 (15) | 0.0344 (6) | |
C22 | 0.4856 (4) | 0.2819 (3) | 0.78413 (15) | 0.0351 (6) | |
C23 | 0.5623 (5) | 0.3377 (4) | 0.83860 (17) | 0.0432 (7) | |
H23A | 0.6004 | 0.4265 | 0.8314 | 0.052* | |
C24 | 0.5825 (5) | 0.2607 (4) | 0.90439 (17) | 0.0478 (8) | |
H24A | 0.6365 | 0.2978 | 0.9405 | 0.057* | |
C25 | 0.5232 (5) | 0.1291 (4) | 0.91687 (16) | 0.0442 (8) | |
C26 | 0.4475 (6) | 0.0748 (4) | 0.86118 (18) | 0.0525 (9) | |
H26A | 0.4070 | −0.0129 | 0.8685 | 0.063* | |
C27 | 0.4311 (5) | 0.1479 (4) | 0.79540 (18) | 0.0471 (8) | |
H27A | 0.3834 | 0.1078 | 0.7583 | 0.057* | |
C28 | 0.5413 (5) | 0.0533 (4) | 0.98769 (17) | 0.0498 (8) | |
H28A | 0.6174 | 0.0827 | 1.0180 | 0.060* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0294 (2) | 0.0318 (2) | 0.02577 (19) | −0.00472 (15) | −0.00555 (13) | 0.00541 (14) |
O1W | 0.0322 (11) | 0.0621 (15) | 0.0343 (11) | −0.0023 (11) | −0.0047 (9) | −0.0101 (10) |
O2W | 0.0312 (10) | 0.0420 (12) | 0.0305 (10) | −0.0074 (9) | −0.0042 (8) | 0.0039 (8) |
O1 | 0.0629 (15) | 0.0392 (12) | 0.0369 (11) | −0.0127 (11) | −0.0139 (10) | 0.0058 (9) |
O2 | 0.0573 (14) | 0.0435 (12) | 0.0338 (11) | −0.0216 (11) | −0.0153 (10) | 0.0154 (9) |
O3 | 0.0327 (11) | 0.0638 (15) | 0.0332 (11) | −0.0054 (11) | −0.0050 (9) | −0.0014 (10) |
O4 | 0.0352 (11) | 0.0336 (11) | 0.0355 (10) | −0.0065 (9) | −0.0097 (8) | 0.0035 (8) |
N1 | 0.0325 (12) | 0.0403 (14) | 0.0376 (13) | −0.0092 (11) | −0.0017 (10) | −0.0001 (10) |
N2 | 0.0339 (12) | 0.0353 (13) | 0.0339 (12) | −0.0093 (11) | −0.0086 (10) | 0.0062 (10) |
C1 | 0.051 (2) | 0.060 (2) | 0.0406 (17) | −0.0186 (18) | 0.0056 (15) | −0.0054 (15) |
C2 | 0.066 (3) | 0.083 (3) | 0.051 (2) | −0.031 (2) | 0.0185 (19) | −0.021 (2) |
C3 | 0.052 (2) | 0.069 (3) | 0.079 (3) | −0.008 (2) | 0.017 (2) | −0.035 (2) |
C4 | 0.0349 (17) | 0.050 (2) | 0.072 (2) | −0.0099 (16) | 0.0013 (16) | −0.0196 (18) |
C5 | 0.045 (2) | 0.038 (2) | 0.109 (4) | 0.0028 (17) | −0.012 (2) | −0.020 (2) |
C6 | 0.049 (2) | 0.0323 (18) | 0.102 (3) | −0.0017 (16) | −0.024 (2) | 0.0034 (19) |
C7 | 0.0375 (16) | 0.0291 (15) | 0.072 (2) | −0.0081 (14) | −0.0220 (15) | 0.0086 (14) |
C8 | 0.056 (2) | 0.0424 (19) | 0.066 (2) | −0.0207 (18) | −0.0305 (18) | 0.0263 (17) |
C9 | 0.058 (2) | 0.053 (2) | 0.0422 (17) | −0.0248 (18) | −0.0189 (15) | 0.0198 (15) |
C10 | 0.0468 (17) | 0.0473 (18) | 0.0349 (15) | −0.0174 (15) | −0.0096 (13) | 0.0085 (13) |
C11 | 0.0281 (13) | 0.0308 (14) | 0.0488 (17) | −0.0072 (12) | −0.0120 (12) | 0.0040 (12) |
C12 | 0.0283 (14) | 0.0363 (16) | 0.0495 (17) | −0.0077 (13) | −0.0038 (12) | −0.0068 (13) |
C13 | 0.0310 (14) | 0.0336 (14) | 0.0322 (14) | −0.0119 (12) | −0.0064 (11) | 0.0043 (11) |
C14 | 0.0354 (15) | 0.0400 (16) | 0.0317 (14) | −0.0129 (13) | −0.0083 (11) | 0.0036 (11) |
C15 | 0.055 (2) | 0.056 (2) | 0.0391 (17) | 0.0019 (17) | −0.0096 (15) | −0.0065 (15) |
C16 | 0.070 (3) | 0.073 (3) | 0.0359 (18) | 0.004 (2) | −0.0074 (17) | −0.0105 (17) |
C17 | 0.059 (2) | 0.071 (2) | 0.0336 (16) | −0.016 (2) | −0.0111 (15) | 0.0014 (16) |
C18 | 0.0441 (18) | 0.062 (2) | 0.0440 (18) | −0.0004 (17) | −0.0145 (14) | 0.0094 (16) |
C19 | 0.0380 (16) | 0.0506 (19) | 0.0343 (15) | −0.0061 (15) | −0.0054 (12) | 0.0017 (13) |
C20 | 0.067 (3) | 0.087 (3) | 0.0363 (18) | −0.002 (2) | −0.0122 (17) | −0.0025 (18) |
C21 | 0.0336 (14) | 0.0362 (15) | 0.0302 (14) | −0.0033 (12) | −0.0019 (11) | 0.0075 (11) |
C22 | 0.0382 (15) | 0.0323 (15) | 0.0317 (14) | −0.0043 (13) | −0.0003 (11) | 0.0079 (11) |
C23 | 0.0530 (19) | 0.0413 (17) | 0.0370 (16) | −0.0155 (15) | −0.0057 (13) | 0.0109 (13) |
C24 | 0.064 (2) | 0.049 (2) | 0.0328 (15) | −0.0188 (18) | −0.0092 (14) | 0.0073 (13) |
C25 | 0.062 (2) | 0.0352 (16) | 0.0314 (15) | −0.0059 (15) | −0.0002 (14) | 0.0073 (12) |
C26 | 0.079 (3) | 0.0394 (18) | 0.0404 (17) | −0.0179 (18) | −0.0041 (17) | 0.0093 (14) |
C27 | 0.067 (2) | 0.0377 (17) | 0.0386 (16) | −0.0162 (17) | −0.0052 (15) | 0.0043 (13) |
C28 | 0.068 (2) | 0.0435 (18) | 0.0340 (16) | −0.0062 (17) | −0.0052 (15) | 0.0090 (13) |
Co1—O2 | 2.069 (2) | C8—H8A | 0.9300 |
Co1—O4 | 2.105 (2) | C9—C10 | 1.400 (4) |
Co1—O1W | 2.109 (2) | C9—H9A | 0.9300 |
Co1—N2 | 2.131 (2) | C10—H10A | 0.9300 |
Co1—N1 | 2.132 (3) | C11—C12 | 1.430 (4) |
Co1—O2W | 2.145 (2) | C13—C14 | 1.499 (4) |
O1W—H1W1 | 0.85 (1) | C14—C15 | 1.379 (5) |
O1W—H1W2 | 0.85 (3) | C14—C19 | 1.386 (4) |
O2W—H2W1 | 0.85 (1) | C15—C16 | 1.378 (5) |
O2W—H2W2 | 0.856 (10) | C15—H15A | 0.9300 |
O1—C21 | 1.246 (4) | C16—C17 | 1.379 (6) |
O2—C21 | 1.263 (4) | C16—H16A | 0.9300 |
O3—C13 | 1.259 (4) | C17—C18 | 1.393 (5) |
O4—C13 | 1.257 (3) | C17—C20 | 1.485 (5) |
N1—C1 | 1.319 (4) | C18—C19 | 1.385 (4) |
N1—C12 | 1.360 (4) | C18—H18A | 0.9300 |
N2—C10 | 1.331 (4) | C19—H19A | 0.9300 |
N2—C11 | 1.354 (4) | C20—C20i | 1.290 (8) |
C1—C2 | 1.399 (5) | C20—H20A | 0.9300 |
C1—H1A | 0.9300 | C21—C22 | 1.508 (4) |
C2—C3 | 1.360 (6) | C22—C23 | 1.381 (5) |
C2—H2A | 0.9300 | C22—C27 | 1.394 (4) |
C3—C4 | 1.394 (6) | C23—C24 | 1.393 (4) |
C3—H3A | 0.9300 | C23—H23A | 0.9300 |
C4—C12 | 1.406 (5) | C24—C25 | 1.392 (5) |
C4—C5 | 1.440 (6) | C24—H24A | 0.9300 |
C5—C6 | 1.340 (6) | C25—C26 | 1.388 (5) |
C5—H5A | 0.9300 | C25—C28 | 1.469 (4) |
C6—C7 | 1.417 (5) | C26—C27 | 1.375 (4) |
C6—H6A | 0.9300 | C26—H26A | 0.9300 |
C7—C8 | 1.394 (5) | C27—H27A | 0.9300 |
C7—C11 | 1.415 (4) | C28—C28ii | 1.327 (7) |
C8—C9 | 1.357 (5) | C28—H28A | 0.9300 |
O2—Co1—O4 | 84.05 (8) | N2—C10—H10A | 118.6 |
O2—Co1—O1W | 92.31 (10) | C9—C10—H10A | 118.6 |
O4—Co1—O1W | 87.44 (9) | N2—C11—C7 | 122.9 (3) |
O2—Co1—N2 | 169.76 (9) | N2—C11—C12 | 117.4 (3) |
O4—Co1—N2 | 100.04 (9) | C7—C11—C12 | 119.7 (3) |
O1W—Co1—N2 | 97.24 (10) | N1—C12—C4 | 123.2 (3) |
O2—Co1—N1 | 93.57 (10) | N1—C12—C11 | 116.8 (3) |
O4—Co1—N1 | 86.75 (9) | C4—C12—C11 | 120.0 (3) |
O1W—Co1—N1 | 171.27 (10) | O4—C13—O3 | 123.8 (3) |
N2—Co1—N1 | 77.39 (10) | O4—C13—C14 | 117.8 (3) |
O2—Co1—O2W | 87.87 (8) | O3—C13—C14 | 118.4 (3) |
O4—Co1—O2W | 169.94 (8) | C15—C14—C19 | 118.6 (3) |
O1W—Co1—O2W | 86.90 (9) | C15—C14—C13 | 119.6 (3) |
N2—Co1—O2W | 88.93 (9) | C19—C14—C13 | 121.8 (3) |
N1—Co1—O2W | 99.76 (9) | C16—C15—C14 | 120.9 (4) |
Co1—O1W—H1W1 | 138 (3) | C16—C15—H15A | 119.5 |
Co1—O1W—H1W2 | 100 (2) | C14—C15—H15A | 119.5 |
H1W1—O1W—H1W2 | 110.2 (17) | C17—C16—C15 | 121.4 (4) |
Co1—O2W—H2W1 | 117 (3) | C17—C16—H16A | 119.3 |
Co1—O2W—H2W2 | 95 (2) | C15—C16—H16A | 119.3 |
H2W1—O2W—H2W2 | 108.6 (16) | C16—C17—C18 | 117.5 (3) |
C21—O2—Co1 | 129.21 (19) | C16—C17—C20 | 118.1 (4) |
C13—O4—Co1 | 119.98 (18) | C18—C17—C20 | 124.3 (4) |
C1—N1—C12 | 118.1 (3) | C19—C18—C17 | 121.3 (3) |
C1—N1—Co1 | 127.6 (2) | C19—C18—H18A | 119.4 |
C12—N1—Co1 | 114.2 (2) | C17—C18—H18A | 119.4 |
C10—N2—C11 | 117.8 (3) | C18—C19—C14 | 120.2 (3) |
C10—N2—Co1 | 128.1 (2) | C18—C19—H19A | 119.9 |
C11—N2—Co1 | 114.14 (19) | C14—C19—H19A | 119.9 |
N1—C1—C2 | 122.4 (4) | C20i—C20—C17 | 127.2 (5) |
N1—C1—H1A | 118.8 | C20i—C20—H20A | 116.4 |
C2—C1—H1A | 118.8 | C17—C20—H20A | 116.4 |
C3—C2—C1 | 119.4 (4) | O1—C21—O2 | 126.3 (3) |
C3—C2—H2A | 120.3 | O1—C21—C22 | 117.5 (3) |
C1—C2—H2A | 120.3 | O2—C21—C22 | 116.2 (3) |
C2—C3—C4 | 120.4 (4) | C23—C22—C27 | 119.4 (3) |
C2—C3—H3A | 119.8 | C23—C22—C21 | 121.2 (3) |
C4—C3—H3A | 119.8 | C27—C22—C21 | 119.3 (3) |
C3—C4—C12 | 116.5 (4) | C22—C23—C24 | 119.9 (3) |
C3—C4—C5 | 125.0 (4) | C22—C23—H23A | 120.1 |
C12—C4—C5 | 118.5 (4) | C24—C23—H23A | 120.1 |
C6—C5—C4 | 121.0 (4) | C25—C24—C23 | 121.0 (3) |
C6—C5—H5A | 119.5 | C25—C24—H24A | 119.5 |
C4—C5—H5A | 119.5 | C23—C24—H24A | 119.5 |
C5—C6—C7 | 122.1 (4) | C26—C25—C24 | 118.0 (3) |
C5—C6—H6A | 119.0 | C26—C25—C28 | 122.3 (3) |
C7—C6—H6A | 119.0 | C24—C25—C28 | 119.6 (3) |
C8—C7—C11 | 117.0 (3) | C27—C26—C25 | 121.4 (3) |
C8—C7—C6 | 124.3 (3) | C27—C26—H26A | 119.3 |
C11—C7—C6 | 118.7 (3) | C25—C26—H26A | 119.3 |
C9—C8—C7 | 120.2 (3) | C26—C27—C22 | 120.2 (3) |
C9—C8—H8A | 119.9 | C26—C27—H27A | 119.9 |
C7—C8—H8A | 119.9 | C22—C27—H27A | 119.9 |
C8—C9—C10 | 119.2 (3) | C28ii—C28—C25 | 125.9 (5) |
C8—C9—H9A | 120.4 | C28ii—C28—H28A | 117.1 |
C10—C9—H9A | 120.4 | C25—C28—H28A | 117.1 |
N2—C10—C9 | 122.9 (3) | ||
O4—Co1—O2—C21 | −157.9 (3) | C8—C7—C11—C12 | −179.0 (3) |
O1W—Co1—O2—C21 | −70.7 (3) | C6—C7—C11—C12 | −0.1 (4) |
N2—Co1—O2—C21 | 88.0 (6) | C1—N1—C12—C4 | −0.9 (4) |
N1—Co1—O2—C21 | 115.8 (3) | Co1—N1—C12—C4 | −177.4 (2) |
O2W—Co1—O2—C21 | 16.1 (3) | C1—N1—C12—C11 | 178.4 (3) |
O2—Co1—O4—C13 | 51.2 (2) | Co1—N1—C12—C11 | 1.9 (3) |
O1W—Co1—O4—C13 | −41.4 (2) | C3—C4—C12—N1 | −0.4 (5) |
N2—Co1—O4—C13 | −138.3 (2) | C5—C4—C12—N1 | 178.9 (3) |
N1—Co1—O4—C13 | 145.2 (2) | C3—C4—C12—C11 | −179.7 (3) |
O2W—Co1—O4—C13 | 14.5 (5) | C5—C4—C12—C11 | −0.3 (5) |
O2—Co1—N1—C1 | 6.0 (3) | N2—C11—C12—N1 | 1.0 (4) |
O4—Co1—N1—C1 | −77.8 (3) | C7—C11—C12—N1 | −178.9 (3) |
N2—Co1—N1—C1 | −178.8 (3) | N2—C11—C12—C4 | −179.7 (3) |
O2W—Co1—N1—C1 | 94.5 (3) | C7—C11—C12—C4 | 0.4 (4) |
O2—Co1—N1—C12 | −177.9 (2) | Co1—O4—C13—O3 | 63.9 (3) |
O4—Co1—N1—C12 | 98.3 (2) | Co1—O4—C13—C14 | −114.4 (2) |
N2—Co1—N1—C12 | −2.8 (2) | O4—C13—C14—C15 | −8.7 (4) |
O2W—Co1—N1—C12 | −89.5 (2) | O3—C13—C14—C15 | 172.8 (3) |
O2—Co1—N2—C10 | −150.0 (4) | O4—C13—C14—C19 | 168.4 (3) |
O4—Co1—N2—C10 | 97.2 (3) | O3—C13—C14—C19 | −10.0 (4) |
O1W—Co1—N2—C10 | 8.5 (3) | C19—C14—C15—C16 | 0.8 (5) |
N1—Co1—N2—C10 | −178.5 (3) | C13—C14—C15—C16 | 178.1 (3) |
O2W—Co1—N2—C10 | −78.2 (3) | C14—C15—C16—C17 | 0.1 (7) |
O2—Co1—N2—C11 | 31.8 (6) | C15—C16—C17—C18 | −1.3 (6) |
O4—Co1—N2—C11 | −81.0 (2) | C15—C16—C17—C20 | 179.4 (4) |
O1W—Co1—N2—C11 | −169.68 (19) | C16—C17—C18—C19 | 1.6 (6) |
N1—Co1—N2—C11 | 3.33 (19) | C20—C17—C18—C19 | −179.1 (4) |
O2W—Co1—N2—C11 | 103.58 (19) | C17—C18—C19—C14 | −0.7 (6) |
C12—N1—C1—C2 | 1.2 (5) | C15—C14—C19—C18 | −0.5 (5) |
Co1—N1—C1—C2 | 177.2 (3) | C13—C14—C19—C18 | −177.7 (3) |
N1—C1—C2—C3 | −0.3 (6) | C16—C17—C20—C20i | −177.1 (6) |
C1—C2—C3—C4 | −1.1 (6) | C18—C17—C20—C20i | 3.6 (9) |
C2—C3—C4—C12 | 1.4 (6) | Co1—O2—C21—O1 | 3.4 (5) |
C2—C3—C4—C5 | −177.9 (4) | Co1—O2—C21—C22 | −174.32 (19) |
C3—C4—C5—C6 | 179.2 (4) | O1—C21—C22—C23 | 176.1 (3) |
C12—C4—C5—C6 | −0.1 (5) | O2—C21—C22—C23 | −6.0 (4) |
C4—C5—C6—C7 | 0.4 (6) | O1—C21—C22—C27 | −6.3 (4) |
C5—C6—C7—C8 | 178.5 (4) | O2—C21—C22—C27 | 171.6 (3) |
C5—C6—C7—C11 | −0.3 (5) | C27—C22—C23—C24 | −0.7 (5) |
C11—C7—C8—C9 | −0.3 (5) | C21—C22—C23—C24 | 176.9 (3) |
C6—C7—C8—C9 | −179.0 (3) | C22—C23—C24—C25 | −1.3 (6) |
C7—C8—C9—C10 | 0.3 (5) | C23—C24—C25—C26 | 1.6 (6) |
C11—N2—C10—C9 | 2.0 (4) | C23—C24—C25—C28 | −178.1 (3) |
Co1—N2—C10—C9 | −176.2 (2) | C24—C25—C26—C27 | 0.0 (6) |
C8—C9—C10—N2 | −1.2 (5) | C28—C25—C26—C27 | 179.7 (4) |
C10—N2—C11—C7 | −1.9 (4) | C25—C26—C27—C22 | −2.0 (6) |
Co1—N2—C11—C7 | 176.5 (2) | C23—C22—C27—C26 | 2.3 (5) |
C10—N2—C11—C12 | 178.1 (3) | C21—C22—C27—C26 | −175.4 (3) |
Co1—N2—C11—C12 | −3.5 (3) | C26—C25—C28—C28ii | −14.3 (7) |
C8—C7—C11—N2 | 1.1 (4) | C24—C25—C28—C28ii | 165.4 (5) |
C6—C7—C11—N2 | 180.0 (3) |
Symmetry codes: (i) −x+2, −y+1, −z+2; (ii) −x+1, −y, −z+2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O2Wiii | 0.85 (1) | 1.90 (1) | 2.749 (3) | 177 (4) |
O1W—H1W2···O3 | 0.85 (3) | 1.83 (3) | 2.653 (3) | 164 (3) |
O2W—H2W1···O3iv | 0.85 (1) | 1.83 (3) | 2.679 (3) | 172 (3) |
O2W—H2W2···O1 | 0.86 (1) | 1.72 (3) | 2.564 (3) | 169 (4) |
O2W—H2W2···O2 | 0.86 (1) | 2.51 (4) | 2.925 (3) | 111 (3) |
Symmetry codes: (iii) −x+1, −y+1, −z+1; (iv) x−1, y, z. |
Experimental details
Crystal data | |
Chemical formula | [Co(C16H10O4)(C12H8N2)H2O)2] |
Mr | 541.41 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 295 |
a, b, c (Å) | 7.5345 (15), 9.2112 (18), 18.524 (4) |
α, β, γ (°) | 88.12 (3), 84.29 (3), 76.38 (3) |
V (Å3) | 1243.2 (5) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.74 |
Crystal size (mm) | 0.36 × 0.24 × 0.12 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID diffractometer |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.811, 0.917 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11895, 5509, 4338 |
Rint | 0.030 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.043, 0.142, 1.01 |
No. of reflections | 5509 |
No. of parameters | 346 |
No. of restraints | 6 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.47, −0.48 |
Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), publCIF (Westrip 2007).
Co1—O2 | 2.069 (2) | Co1—N2 | 2.131 (2) |
Co1—O4 | 2.105 (2) | Co1—N1 | 2.132 (3) |
Co1—O1W | 2.109 (2) | Co1—O2W | 2.145 (2) |
O2—Co1—O4 | 84.05 (8) | O1W—Co1—N1 | 171.27 (10) |
O2—Co1—O1W | 92.31 (10) | N2—Co1—N1 | 77.39 (10) |
O4—Co1—O1W | 87.44 (9) | O2—Co1—O2W | 87.87 (8) |
O2—Co1—N2 | 169.76 (9) | O4—Co1—O2W | 169.94 (8) |
O4—Co1—N2 | 100.04 (9) | O1W—Co1—O2W | 86.90 (9) |
O1W—Co1—N2 | 97.24 (10) | N2—Co1—O2W | 88.93 (9) |
O2—Co1—N1 | 93.57 (10) | N1—Co1—O2W | 99.76 (9) |
O4—Co1—N1 | 86.75 (9) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O2Wi | 0.85 (1) | 1.900 (11) | 2.749 (3) | 177 (4) |
O1W—H1W2···O3 | 0.85 (3) | 1.83 (3) | 2.653 (3) | 164 (3) |
O2W—H2W1···O3ii | 0.85 (1) | 1.83 (3) | 2.679 (3) | 172 (3) |
O2W—H2W2···O1 | 0.856 (10) | 1.72 (3) | 2.564 (3) | 169 (4) |
O2W—H2W2···O2 | 0.856 (10) | 2.51 (4) | 2.925 (3) | 111 (3) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x−1, y, z. |
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Many new complexes have been synthesized using polycarboxylates to combine with specific transition metal ions by introdcing neutral N-heterocyclic ligands (Wang et al., 2004; Wang, Qin et al., 2006). We report here the synthesis and structure of a new one-dimensional cobalt complex (Fig. 1).
The complex is an infinite one-dimensional chain polymer with a CoII ion, two half of trans-stilbene-4,4'-dicarboxylato ligands, a 1,10-phenanthroline and two coordinated water molecules in the asymmetric unit. Each CoII ion is in a distorted octahedral geometry. The [Co(1,10-phenanthroline)(H2O)2] units are connected by trans-stilbene-4,4'-dicarboxylato bridges with bis-dentate mode to form an one-dimensional zigzag chain structure. The chains are further interconnected through intermolecular hydrogen bonds and π–π stacking interactions between one of the rings of the 1,10-phenanthroline ligand (C7–C10/N2/C11) and symmetry-related ring at (1 - x, 2 - y, 1 - z), with a centroid-to-centroid distance of 3.6153 (8) Å into three-dimensional supramolecular network (Table 2 and Fig. 2). The structure contains voids of about 105.00 A3 and there is no solvent molecules occupied.