Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807048532/cv2313sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807048532/cv2313Isup2.hkl |
CCDC reference: 667144
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- R factor = 0.047
- wR factor = 0.136
- Data-to-parameter ratio = 16.1
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 1.05
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 1.053 Tmax scaled 0.926 Tmin scaled 0.895 PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT794_ALERT_5_G Check Predicted Bond Valency for Co1 (2) 1.72 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 3
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 5 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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
The ligand L was synthesized according to the literature (Liu et al., 2007). A mixture of Co(NO3)2.6H2O (0.11 g, 0.4 mmol), H3BTC (0.10 g, 0.45 mmol), L (0.10 g, 0.4 mmol) and water (7 ml) was stirred for 10 min in air. The mixture was sealed in a Teflon reactor (15 ml) and heated at 180 °C for 3 days. After the mixture had been cooled to room temperature at 10 °C.h-1, purple crystals of (I) were obtained. Yield: 30%.
The C-bound and hydroxy H-atoms were geometrically positioned (C—H 0.93–0.97 Å, O—H 0.82 Å) and refined using a riding model, with Uiso = 1.2–1.5Ueq (C, O). Water H atoms were located in a difference Fourier map and refined as riding atoms with Uiso(H) = 1.5Ueq(O).
As part of an investigation of the transition metal application there is a need to prepare further examples of these compounds. In this paper, the structure of the title compound, (I), is described.
As shown in Fig. 1, the CoII ions is coordinated by two oxygen atoms from two HBTC anions and two nitrogen atoms from two L ligands. Each CoII cation has a distorted tetrahedral coordination geometry. As illustrated in Fig. 2, each L ligand in (I) coordinates to two CoII cations, thus acting as a bridging bidentate ligand. The CoII cations are bridged by HBTC anions and L ligands to form a double-stranded chain, with the interchain Co···Co distance of 9.072 (6) Å. The hydroxyl groups of adjacent HBTC anions are involved in hydrogen bonding interactions. There also exist face-to-face π-π interactions between the benzene rings of L ligands of adjacent double-stranded chains (with centroid-to-centriod distance of 3.905 (2) Å, and average face-to-face distances of 3.427 (3) Å). These noncovalent interactions connect the whole structure to a 3-D supramolecular framework (Fig. 3). The lattice water molecule connects with HBTC anion via hydrogen bond.
For related crystal structures, see Liu et al. (2007) and Xie et al. (2007).
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 (Sheldrick, 1990); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
[Co(C9H4O6)(C14H14N4)]·H2O | F(000) = 1076 |
Mr = 523.36 | Dx = 1.610 Mg m−3 |
Monoclinic, P21/n | Melting point: not measured K |
Hall symbol: -P 2yn | Mo Kα radiation, λ = 0.71069 Å |
a = 7.8535 (4) Å | Cell parameters from 3606 reflections |
b = 16.5308 (7) Å | θ = 1.7–28.3° |
c = 16.7344 (8) Å | µ = 0.85 mm−1 |
β = 96.350 (1)° | T = 293 K |
V = 2159.21 (18) Å3 | Block, purple |
Z = 4 | 0.13 × 0.11 × 0.09 mm |
Bruker APEX CCD area-detector diffractometer | 5192 independent reflections |
Radiation source: fine-focus sealed tube | 3606 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
ω scans | θmax = 28.3°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→10 |
Tmin = 0.85, Tmax = 0.88 | k = −22→11 |
13208 measured reflections | l = −20→21 |
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)] = 0.047 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.136 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.069P)2] where P = (Fo2 + 2Fc2)/3 |
5192 reflections | (Δ/σ)max = 0.001 |
322 parameters | Δρmax = 0.53 e Å−3 |
3 restraints | Δρmin = −0.76 e Å−3 |
[Co(C9H4O6)(C14H14N4)]·H2O | V = 2159.21 (18) Å3 |
Mr = 523.36 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 7.8535 (4) Å | µ = 0.85 mm−1 |
b = 16.5308 (7) Å | T = 293 K |
c = 16.7344 (8) Å | 0.13 × 0.11 × 0.09 mm |
β = 96.350 (1)° |
Bruker APEX CCD area-detector diffractometer | 5192 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3606 reflections with I > 2σ(I) |
Tmin = 0.85, Tmax = 0.88 | Rint = 0.046 |
13208 measured reflections |
R[F2 > 2σ(F2)] = 0.047 | 3 restraints |
wR(F2) = 0.136 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | Δρmax = 0.53 e Å−3 |
5192 reflections | Δρmin = −0.76 e Å−3 |
322 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 | 0.91070 (5) | 0.18840 (2) | 0.78370 (2) | 0.02526 (13) | |
C1 | 0.9365 (4) | 0.31872 (16) | 0.58113 (17) | 0.0268 (6) | |
C2 | 1.0894 (4) | 0.36035 (17) | 0.57876 (16) | 0.0280 (6) | |
H2 | 1.1715 | 0.3605 | 0.6233 | 0.034* | |
C3 | 1.1189 (3) | 0.40177 (17) | 0.50920 (16) | 0.0270 (6) | |
C4 | 0.9958 (3) | 0.40212 (17) | 0.44239 (16) | 0.0267 (6) | |
H4 | 1.0159 | 0.4304 | 0.3963 | 0.032* | |
C5 | 0.8430 (3) | 0.36021 (17) | 0.44470 (16) | 0.0261 (6) | |
C6 | 0.8149 (4) | 0.31896 (17) | 0.51446 (17) | 0.0280 (6) | |
H6 | 0.7127 | 0.2910 | 0.5164 | 0.034* | |
C7 | 0.9062 (4) | 0.26952 (17) | 0.65377 (17) | 0.0295 (6) | |
C8 | 1.2853 (4) | 0.44426 (18) | 0.50588 (17) | 0.0321 (7) | |
C9 | 0.7107 (4) | 0.35829 (17) | 0.37216 (16) | 0.0291 (6) | |
C10 | 0.3481 (4) | −0.02287 (17) | 0.62968 (18) | 0.0298 (6) | |
C11 | 0.2631 (4) | 0.04946 (18) | 0.61044 (18) | 0.0315 (7) | |
H11 | 0.2456 | 0.0857 | 0.6512 | 0.038* | |
C12 | 0.2038 (4) | 0.06864 (18) | 0.53144 (18) | 0.0322 (7) | |
C13 | 0.2269 (4) | 0.01358 (19) | 0.47063 (19) | 0.0359 (7) | |
H13 | 0.1864 | 0.0254 | 0.4176 | 0.043* | |
C14 | 0.3102 (4) | −0.0589 (2) | 0.48938 (19) | 0.0389 (7) | |
H14 | 0.3265 | −0.0954 | 0.4486 | 0.047* | |
C15 | 0.3694 (4) | −0.07736 (19) | 0.56790 (19) | 0.0338 (7) | |
H15 | 0.4240 | −0.1265 | 0.5798 | 0.041* | |
C16 | 0.4167 (4) | −0.04058 (18) | 0.71596 (18) | 0.0348 (7) | |
H16A | 0.3418 | −0.0165 | 0.7517 | 0.042* | |
H16B | 0.4181 | −0.0986 | 0.7247 | 0.042* | |
C17 | 0.1128 (4) | 0.1487 (2) | 0.5173 (2) | 0.0424 (8) | |
H17A | −0.0070 | 0.1414 | 0.5246 | 0.051* | |
H17B | 0.1610 | 0.1869 | 0.5576 | 0.051* | |
C18 | 0.6342 (4) | 0.06991 (18) | 0.74057 (18) | 0.0334 (7) | |
H18 | 0.5559 | 0.1122 | 0.7343 | 0.040* | |
C19 | 0.7410 (4) | −0.05168 (19) | 0.74705 (17) | 0.0350 (7) | |
H19 | 0.7518 | −0.1077 | 0.7463 | 0.042* | |
C20 | 0.8687 (4) | 0.00252 (18) | 0.76034 (19) | 0.0354 (7) | |
H20 | 0.9845 | −0.0100 | 0.7706 | 0.042* | |
C21 | 0.2584 (4) | 0.22522 (18) | 0.41509 (18) | 0.0315 (6) | |
H21 | 0.3587 | 0.2352 | 0.4486 | 0.038* | |
C22 | 0.0010 (4) | 0.18314 (19) | 0.3727 (2) | 0.0370 (7) | |
H22 | −0.1069 | 0.1596 | 0.3705 | 0.044* | |
C23 | 0.0662 (4) | 0.22343 (19) | 0.31230 (19) | 0.0347 (7) | |
H23 | 0.0103 | 0.2319 | 0.2610 | 0.042* | |
N1 | 0.8011 (3) | 0.07952 (15) | 0.75631 (14) | 0.0309 (5) | |
N2 | 0.5918 (3) | −0.00812 (14) | 0.73483 (14) | 0.0293 (5) | |
N3 | 0.1237 (3) | 0.18368 (15) | 0.43720 (16) | 0.0343 (6) | |
N4 | 0.2298 (3) | 0.24994 (14) | 0.33969 (14) | 0.0278 (5) | |
O1 | 0.7668 (3) | 0.23374 (14) | 0.65682 (13) | 0.0428 (6) | |
O2 | 1.0259 (3) | 0.26347 (13) | 0.71064 (12) | 0.0371 (5) | |
O3 | 1.4018 (3) | 0.43829 (16) | 0.56198 (14) | 0.0511 (6) | |
O4 | 1.2972 (3) | 0.48619 (14) | 0.44202 (13) | 0.0450 (6) | |
H4A | 1.3920 | 0.5075 | 0.4448 | 0.068* | |
O5 | 0.7363 (3) | 0.39334 (15) | 0.30987 (12) | 0.0443 (6) | |
O6 | 0.5753 (3) | 0.31807 (13) | 0.38107 (13) | 0.0372 (5) | |
O1W | 0.4422 (6) | 0.2569 (4) | 0.5980 (4) | 0.1444 (18) | |
H1A | 0.559 (4) | 0.247 (5) | 0.610 (6) | 0.217* | |
H1B | 0.436 (11) | 0.3110 (17) | 0.588 (6) | 0.217* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0260 (2) | 0.0274 (2) | 0.0221 (2) | −0.00004 (16) | 0.00142 (15) | 0.00103 (15) |
C1 | 0.0325 (15) | 0.0245 (15) | 0.0236 (14) | −0.0015 (11) | 0.0038 (12) | 0.0011 (11) |
C2 | 0.0306 (15) | 0.0314 (16) | 0.0215 (14) | −0.0007 (12) | 0.0004 (11) | 0.0005 (11) |
C3 | 0.0266 (14) | 0.0291 (15) | 0.0256 (15) | −0.0028 (11) | 0.0041 (11) | −0.0011 (11) |
C4 | 0.0309 (15) | 0.0278 (15) | 0.0218 (14) | −0.0019 (12) | 0.0037 (11) | 0.0037 (11) |
C5 | 0.0279 (14) | 0.0277 (15) | 0.0225 (14) | −0.0027 (11) | 0.0021 (11) | 0.0004 (11) |
C6 | 0.0294 (15) | 0.0301 (16) | 0.0243 (14) | −0.0047 (12) | 0.0022 (12) | −0.0010 (11) |
C7 | 0.0393 (17) | 0.0258 (15) | 0.0242 (15) | −0.0006 (12) | 0.0073 (12) | 0.0025 (11) |
C8 | 0.0366 (16) | 0.0341 (17) | 0.0262 (15) | −0.0057 (13) | 0.0056 (13) | −0.0011 (12) |
C9 | 0.0306 (15) | 0.0314 (16) | 0.0243 (15) | −0.0008 (12) | −0.0010 (12) | −0.0018 (12) |
C10 | 0.0276 (15) | 0.0259 (15) | 0.0364 (17) | −0.0063 (11) | 0.0060 (12) | 0.0002 (12) |
C11 | 0.0348 (16) | 0.0275 (16) | 0.0331 (16) | −0.0043 (12) | 0.0079 (13) | −0.0022 (12) |
C12 | 0.0295 (15) | 0.0317 (16) | 0.0365 (17) | −0.0035 (12) | 0.0089 (13) | 0.0045 (13) |
C13 | 0.0352 (16) | 0.0417 (19) | 0.0312 (17) | −0.0066 (14) | 0.0051 (13) | 0.0014 (13) |
C14 | 0.0384 (17) | 0.0385 (19) | 0.0414 (19) | −0.0047 (14) | 0.0115 (15) | −0.0089 (14) |
C15 | 0.0282 (15) | 0.0305 (16) | 0.0434 (18) | −0.0009 (12) | 0.0073 (13) | −0.0041 (13) |
C16 | 0.0385 (17) | 0.0290 (16) | 0.0369 (17) | −0.0050 (13) | 0.0045 (14) | 0.0038 (13) |
C17 | 0.0408 (18) | 0.045 (2) | 0.044 (2) | 0.0059 (15) | 0.0176 (15) | 0.0125 (15) |
C18 | 0.0359 (17) | 0.0256 (16) | 0.0373 (17) | 0.0034 (12) | −0.0019 (13) | 0.0000 (12) |
C19 | 0.0400 (18) | 0.0276 (17) | 0.0373 (17) | 0.0057 (13) | 0.0032 (14) | −0.0014 (13) |
C20 | 0.0348 (17) | 0.0324 (17) | 0.0388 (17) | 0.0069 (13) | 0.0036 (13) | −0.0017 (13) |
C21 | 0.0261 (15) | 0.0322 (16) | 0.0362 (17) | 0.0004 (12) | 0.0033 (12) | 0.0010 (13) |
C22 | 0.0245 (15) | 0.0405 (19) | 0.0454 (19) | −0.0068 (13) | 0.0017 (13) | 0.0048 (14) |
C23 | 0.0289 (16) | 0.0371 (18) | 0.0374 (17) | −0.0015 (13) | 0.0002 (13) | 0.0003 (13) |
N1 | 0.0325 (13) | 0.0291 (14) | 0.0303 (13) | −0.0005 (10) | −0.0002 (10) | 0.0002 (10) |
N2 | 0.0329 (13) | 0.0232 (13) | 0.0313 (13) | −0.0001 (10) | 0.0021 (10) | −0.0018 (10) |
N3 | 0.0304 (13) | 0.0325 (14) | 0.0412 (16) | −0.0005 (11) | 0.0088 (11) | 0.0078 (11) |
N4 | 0.0252 (12) | 0.0279 (13) | 0.0305 (13) | −0.0006 (10) | 0.0037 (10) | 0.0000 (10) |
O1 | 0.0420 (13) | 0.0486 (14) | 0.0372 (13) | −0.0145 (11) | 0.0020 (10) | 0.0138 (10) |
O2 | 0.0379 (12) | 0.0453 (14) | 0.0268 (11) | −0.0039 (10) | −0.0021 (9) | 0.0091 (9) |
O3 | 0.0370 (13) | 0.0736 (18) | 0.0401 (14) | −0.0219 (12) | −0.0072 (11) | 0.0147 (12) |
O4 | 0.0385 (12) | 0.0586 (15) | 0.0377 (13) | −0.0183 (11) | 0.0027 (10) | 0.0104 (11) |
O5 | 0.0459 (13) | 0.0598 (15) | 0.0258 (12) | −0.0092 (11) | −0.0016 (10) | 0.0140 (10) |
O6 | 0.0311 (11) | 0.0514 (14) | 0.0279 (11) | −0.0125 (10) | −0.0025 (9) | 0.0017 (9) |
O1W | 0.109 (3) | 0.190 (5) | 0.132 (4) | 0.003 (4) | 0.006 (3) | 0.019 (4) |
Co1—O6i | 1.968 (2) | C14—C15 | 1.379 (4) |
Co1—O2 | 2.024 (2) | C14—H14 | 0.9300 |
Co1—N1 | 2.026 (2) | C15—H15 | 0.9300 |
Co1—N4i | 2.057 (2) | C16—N2 | 1.477 (4) |
C1—C6 | 1.386 (4) | C16—H16A | 0.9700 |
C1—C2 | 1.388 (4) | C16—H16B | 0.9700 |
C1—C7 | 1.503 (4) | C17—N3 | 1.471 (4) |
C2—C3 | 1.392 (4) | C17—H17A | 0.9700 |
C2—H2 | 0.9300 | C17—H17B | 0.9700 |
C3—C4 | 1.395 (4) | C18—N1 | 1.318 (4) |
C3—C8 | 1.490 (4) | C18—N2 | 1.333 (4) |
C4—C5 | 1.390 (4) | C18—H18 | 0.9300 |
C4—H4 | 0.9300 | C19—C20 | 1.345 (4) |
C5—C6 | 1.390 (4) | C19—N2 | 1.371 (4) |
C5—C9 | 1.508 (4) | C19—H19 | 0.9300 |
C6—H6 | 0.9300 | C20—N1 | 1.378 (4) |
C7—O1 | 1.250 (3) | C20—H20 | 0.9300 |
C7—O2 | 1.266 (4) | C21—N4 | 1.322 (4) |
C8—O3 | 1.240 (4) | C21—N3 | 1.346 (4) |
C8—O4 | 1.286 (3) | C21—H21 | 0.9300 |
C9—O5 | 1.228 (3) | C22—C23 | 1.356 (4) |
C9—O6 | 1.277 (3) | C22—N3 | 1.366 (4) |
C10—C11 | 1.390 (4) | C22—H22 | 0.9300 |
C10—C15 | 1.395 (4) | C23—N4 | 1.387 (4) |
C10—C16 | 1.513 (4) | C23—H23 | 0.9300 |
C11—C12 | 1.389 (4) | N4—Co1ii | 2.057 (2) |
C11—H11 | 0.9300 | O4—H4A | 0.8200 |
C12—C13 | 1.392 (4) | O6—Co1ii | 1.968 (2) |
C12—C17 | 1.511 (4) | O1W—H1A | 0.93 (2) |
C13—C14 | 1.384 (4) | O1W—H1B | 0.91 (2) |
C13—H13 | 0.9300 | ||
O6i—Co1—O2 | 103.70 (9) | C14—C15—H15 | 119.7 |
O6i—Co1—N1 | 111.27 (9) | C10—C15—H15 | 119.7 |
O2—Co1—N1 | 127.96 (9) | N2—C16—C10 | 111.0 (2) |
O6i—Co1—N4i | 94.21 (9) | N2—C16—H16A | 109.4 |
O2—Co1—N4i | 110.41 (9) | C10—C16—H16A | 109.4 |
N1—Co1—N4i | 104.23 (9) | N2—C16—H16B | 109.4 |
C6—C1—C2 | 119.8 (3) | C10—C16—H16B | 109.4 |
C6—C1—C7 | 119.7 (3) | H16A—C16—H16B | 108.0 |
C2—C1—C7 | 120.4 (3) | N3—C17—C12 | 114.4 (3) |
C1—C2—C3 | 119.5 (3) | N3—C17—H17A | 108.7 |
C1—C2—H2 | 120.3 | C12—C17—H17A | 108.7 |
C3—C2—H2 | 120.3 | N3—C17—H17B | 108.7 |
C2—C3—C4 | 120.5 (3) | C12—C17—H17B | 108.7 |
C2—C3—C8 | 119.4 (3) | H17A—C17—H17B | 107.6 |
C4—C3—C8 | 120.1 (2) | N1—C18—N2 | 111.5 (3) |
C5—C4—C3 | 120.0 (2) | N1—C18—H18 | 124.3 |
C5—C4—H4 | 120.0 | N2—C18—H18 | 124.3 |
C3—C4—H4 | 120.0 | C20—C19—N2 | 106.5 (3) |
C4—C5—C6 | 119.0 (3) | C20—C19—H19 | 126.7 |
C4—C5—C9 | 120.5 (2) | N2—C19—H19 | 126.7 |
C6—C5—C9 | 120.4 (2) | C19—C20—N1 | 109.3 (3) |
C1—C6—C5 | 121.2 (3) | C19—C20—H20 | 125.3 |
C1—C6—H6 | 119.4 | N1—C20—H20 | 125.3 |
C5—C6—H6 | 119.4 | N4—C21—N3 | 111.4 (3) |
O1—C7—O2 | 120.9 (3) | N4—C21—H21 | 124.3 |
O1—C7—C1 | 120.5 (3) | N3—C21—H21 | 124.3 |
O2—C7—C1 | 118.7 (3) | C23—C22—N3 | 107.1 (3) |
O3—C8—O4 | 123.8 (3) | C23—C22—H22 | 126.4 |
O3—C8—C3 | 120.7 (3) | N3—C22—H22 | 126.4 |
O4—C8—C3 | 115.5 (3) | C22—C23—N4 | 108.7 (3) |
O5—C9—O6 | 124.1 (3) | C22—C23—H23 | 125.6 |
O5—C9—C5 | 120.7 (3) | N4—C23—H23 | 125.6 |
O6—C9—C5 | 115.2 (2) | C18—N1—C20 | 105.5 (2) |
C11—C10—C15 | 118.5 (3) | C18—N1—Co1 | 122.7 (2) |
C11—C10—C16 | 119.9 (3) | C20—N1—Co1 | 131.2 (2) |
C15—C10—C16 | 121.5 (3) | C18—N2—C19 | 107.1 (2) |
C12—C11—C10 | 121.2 (3) | C18—N2—C16 | 125.9 (2) |
C12—C11—H11 | 119.4 | C19—N2—C16 | 126.9 (2) |
C10—C11—H11 | 119.4 | C21—N3—C22 | 107.0 (3) |
C11—C12—C13 | 119.3 (3) | C21—N3—C17 | 125.3 (3) |
C11—C12—C17 | 116.9 (3) | C22—N3—C17 | 127.6 (3) |
C13—C12—C17 | 123.8 (3) | C21—N4—C23 | 105.7 (2) |
C14—C13—C12 | 119.8 (3) | C21—N4—Co1ii | 122.36 (19) |
C14—C13—H13 | 120.1 | C23—N4—Co1ii | 131.9 (2) |
C12—C13—H13 | 120.1 | C7—O2—Co1 | 99.08 (17) |
C15—C14—C13 | 120.6 (3) | C8—O4—H4A | 109.5 |
C15—C14—H14 | 119.7 | C9—O6—Co1ii | 114.27 (18) |
C13—C14—H14 | 119.7 | H1A—O1W—H1B | 104 (4) |
C14—C15—C10 | 120.5 (3) | ||
C6—C1—C2—C3 | −0.1 (4) | C13—C12—C17—N3 | −28.7 (4) |
C7—C1—C2—C3 | 176.4 (3) | N2—C19—C20—N1 | −0.2 (3) |
C1—C2—C3—C4 | 0.4 (4) | N3—C22—C23—N4 | −0.6 (4) |
C1—C2—C3—C8 | −178.1 (3) | N2—C18—N1—C20 | 0.3 (3) |
C2—C3—C4—C5 | −0.6 (4) | N2—C18—N1—Co1 | −171.73 (18) |
C8—C3—C4—C5 | 177.9 (3) | C19—C20—N1—C18 | −0.1 (3) |
C3—C4—C5—C6 | 0.6 (4) | C19—C20—N1—Co1 | 171.1 (2) |
C3—C4—C5—C9 | −178.4 (2) | O6i—Co1—N1—C18 | 130.6 (2) |
C2—C1—C6—C5 | 0.1 (4) | O2—Co1—N1—C18 | −100.6 (2) |
C7—C1—C6—C5 | −176.4 (3) | N4i—Co1—N1—C18 | 30.3 (3) |
C4—C5—C6—C1 | −0.3 (4) | O6i—Co1—N1—C20 | −39.2 (3) |
C9—C5—C6—C1 | 178.7 (3) | O2—Co1—N1—C20 | 89.6 (3) |
C6—C1—C7—O1 | −5.4 (4) | N4i—Co1—N1—C20 | −139.6 (3) |
C2—C1—C7—O1 | 178.1 (3) | N1—C18—N2—C19 | −0.5 (3) |
C6—C1—C7—O2 | 172.9 (3) | N1—C18—N2—C16 | −178.5 (3) |
C2—C1—C7—O2 | −3.7 (4) | C20—C19—N2—C18 | 0.4 (3) |
C2—C3—C8—O3 | 5.2 (4) | C20—C19—N2—C16 | 178.4 (3) |
C4—C3—C8—O3 | −173.4 (3) | C10—C16—N2—C18 | 69.2 (4) |
C2—C3—C8—O4 | −174.8 (3) | C10—C16—N2—C19 | −108.5 (3) |
C4—C3—C8—O4 | 6.6 (4) | N4—C21—N3—C22 | −1.1 (3) |
C4—C5—C9—O5 | 0.4 (4) | N4—C21—N3—C17 | −179.2 (3) |
C6—C5—C9—O5 | −178.6 (3) | C23—C22—N3—C21 | 1.0 (4) |
C4—C5—C9—O6 | −179.9 (3) | C23—C22—N3—C17 | 179.0 (3) |
C6—C5—C9—O6 | 1.1 (4) | C12—C17—N3—C21 | −80.6 (4) |
C15—C10—C11—C12 | −1.6 (4) | C12—C17—N3—C22 | 101.7 (4) |
C16—C10—C11—C12 | 177.8 (3) | N3—C21—N4—C23 | 0.8 (3) |
C10—C11—C12—C13 | 1.4 (4) | N3—C21—N4—Co1ii | −177.61 (19) |
C10—C11—C12—C17 | 179.8 (3) | C22—C23—N4—C21 | −0.1 (3) |
C11—C12—C13—C14 | −0.9 (4) | C22—C23—N4—Co1ii | 178.1 (2) |
C17—C12—C13—C14 | −179.2 (3) | O1—C7—O2—Co1 | 0.7 (3) |
C12—C13—C14—C15 | 0.6 (4) | C1—C7—O2—Co1 | −177.5 (2) |
C13—C14—C15—C10 | −0.8 (4) | O6i—Co1—O2—C7 | −174.51 (17) |
C11—C10—C15—C14 | 1.3 (4) | N1—Co1—O2—C7 | 53.9 (2) |
C16—C10—C15—C14 | −178.1 (3) | N4i—Co1—O2—C7 | −74.65 (19) |
C11—C10—C16—N2 | −87.8 (3) | O5—C9—O6—Co1ii | 2.9 (4) |
C15—C10—C16—N2 | 91.4 (3) | C5—C9—O6—Co1ii | −176.79 (18) |
C11—C12—C17—N3 | 152.9 (3) |
Symmetry codes: (i) x+1/2, −y+1/2, z+1/2; (ii) x−1/2, −y+1/2, z−1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1A···O1 | 0.93 (2) | 1.74 (3) | 2.657 (5) | 166 (9) |
O4—H4A···O3iii | 0.82 | 1.87 | 2.680 (3) | 173 |
Symmetry code: (iii) −x+3, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Co(C9H4O6)(C14H14N4)]·H2O |
Mr | 523.36 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 7.8535 (4), 16.5308 (7), 16.7344 (8) |
β (°) | 96.350 (1) |
V (Å3) | 2159.21 (18) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.85 |
Crystal size (mm) | 0.13 × 0.11 × 0.09 |
Data collection | |
Diffractometer | Bruker APEX CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.85, 0.88 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13208, 5192, 3606 |
Rint | 0.046 |
(sin θ/λ)max (Å−1) | 0.667 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.047, 0.136, 1.04 |
No. of reflections | 5192 |
No. of parameters | 322 |
No. of restraints | 3 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.53, −0.76 |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Sheldrick, 1990).
Co1—O6i | 1.968 (2) | Co1—N1 | 2.026 (2) |
Co1—O2 | 2.024 (2) | Co1—N4i | 2.057 (2) |
O6i—Co1—O2 | 103.70 (9) | O6i—Co1—N4i | 94.21 (9) |
O6i—Co1—N1 | 111.27 (9) | O2—Co1—N4i | 110.41 (9) |
O2—Co1—N1 | 127.96 (9) | N1—Co1—N4i | 104.23 (9) |
Symmetry code: (i) x+1/2, −y+1/2, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1A···O1 | 0.93 (2) | 1.74 (3) | 2.657 (5) | 166 (9) |
O4—H4A···O3ii | 0.82 | 1.87 | 2.680 (3) | 172.5 |
Symmetry code: (ii) −x+3, −y+1, −z+1. |
As part of an investigation of the transition metal application there is a need to prepare further examples of these compounds. In this paper, the structure of the title compound, (I), is described.
As shown in Fig. 1, the CoII ions is coordinated by two oxygen atoms from two HBTC anions and two nitrogen atoms from two L ligands. Each CoII cation has a distorted tetrahedral coordination geometry. As illustrated in Fig. 2, each L ligand in (I) coordinates to two CoII cations, thus acting as a bridging bidentate ligand. The CoII cations are bridged by HBTC anions and L ligands to form a double-stranded chain, with the interchain Co···Co distance of 9.072 (6) Å. The hydroxyl groups of adjacent HBTC anions are involved in hydrogen bonding interactions. There also exist face-to-face π-π interactions between the benzene rings of L ligands of adjacent double-stranded chains (with centroid-to-centriod distance of 3.905 (2) Å, and average face-to-face distances of 3.427 (3) Å). These noncovalent interactions connect the whole structure to a 3-D supramolecular framework (Fig. 3). The lattice water molecule connects with HBTC anion via hydrogen bond.