Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807056826/hb2627sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807056826/hb2627Isup2.hkl |
CCDC reference: 672718
Key indicators
- Single-crystal X-ray study
- T = 292 K
- Mean (C-C) = 0.006 Å
- R factor = 0.047
- wR factor = 0.114
- Data-to-parameter ratio = 12.4
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT094_ALERT_2_B Ratio of Maximum / Minimum Residual Density .... 4.21
Alert level C PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 4 PLAT333_ALERT_2_C Large Average Benzene C-C Dist. C4 -C18 1.43 Ang. PLAT350_ALERT_3_C Short C-H Bond (0.96A) C30 - H30 ... 0.84 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Co1 (9) 1.65
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For related structures, see Li et al. (2006, 2007). For the ligand synthesis, see Dickeson & Summers (1970).
The Dppz ligand was synthesized by the literature method of Dickeson & Summers (1970). A mixture of CoCl2.2H2O (0.3 mmol), Dppz (0.1 mmol) and benzene-1,4-dicarboxylic acid (0.3 mmol) in 30 ml of distilled water was stirred thoroughly for 1 h at ambient temperature. The pH value was adjusted to about 7.5 with NaOH aqueous solution. The suspension was sealed in a Teflon-lined stainless reaction vessel (40 ml) and heated at 443 K for 5 days. The vessel was cooled slowly to room temperature at a rate of 10 K h-1 before opening, and purple blocks of (I) were recovered.
The water H atoms were located in a difference map and freely refined. The C-bound H atoms were placed geometrically (C—H = 0.93 Å) and refined as riding with Uiso(H)= 1.2Ueq(carrier). The highest difference peak is 1.05Å from H2B.
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; 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: SHELXTL-Plus.
[Co(C8H4O4)(C18H10N4)(H2O)] | F(000) = 1068.0 |
Mr = 523.36 | Dx = 1.587 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 1368 reflections |
a = 10.5218 (19) Å | θ = 2.3–26.1° |
b = 11.742 (2) Å | µ = 0.83 mm−1 |
c = 18.077 (3) Å | T = 292 K |
β = 101.281 (4)° | Block, purple |
V = 2190.2 (7) Å3 | 0.47 × 0.21 × 0.10 mm |
Z = 4 |
Bruker APEXII diffractometer | 4317 independent reflections |
Radiation source: fine-focus sealed tube | 2417 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.059 |
Detector resolution: 0 pixels mm-1 | θmax = 26.0°, θmin = 2.1° |
ω scans | h = −12→10 |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | k = −14→11 |
Tmin = 0.815, Tmax = 0.924 | l = −20→22 |
11590 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)] = 0.047 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.114 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.88 | w = 1/[σ2(Fo2) + (0.0475P)2] where P = (Fo2 + 2Fc2)/3 |
4317 reflections | (Δ/σ)max = 0.001 |
349 parameters | Δρmax = 1.70 e Å−3 |
0 restraints | Δρmin = −0.40 e Å−3 |
[Co(C8H4O4)(C18H10N4)(H2O)] | V = 2190.2 (7) Å3 |
Mr = 523.36 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.5218 (19) Å | µ = 0.83 mm−1 |
b = 11.742 (2) Å | T = 292 K |
c = 18.077 (3) Å | 0.47 × 0.21 × 0.10 mm |
β = 101.281 (4)° |
Bruker APEXII diffractometer | 4317 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | 2417 reflections with I > 2σ(I) |
Tmin = 0.815, Tmax = 0.924 | Rint = 0.059 |
11590 measured reflections |
R[F2 > 2σ(F2)] = 0.047 | 0 restraints |
wR(F2) = 0.114 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.88 | Δρmax = 1.70 e Å−3 |
4317 reflections | Δρmin = −0.40 e Å−3 |
349 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 | 0.49412 (5) | 0.06855 (4) | 0.63798 (3) | 0.03467 (18) | |
O1 | 0.3496 (3) | −0.0366 (2) | 0.57392 (15) | 0.0440 (7) | |
O2 | 0.2835 (3) | 0.1061 (2) | 0.63506 (15) | 0.0487 (8) | |
O3 | 0.6371 (3) | 0.0100 (3) | 0.58260 (19) | 0.0450 (8) | |
N1 | 0.5516 (3) | −0.0670 (3) | 0.72031 (16) | 0.0367 (8) | |
C5 | 0.6497 (3) | −0.0620 (3) | 0.9301 (2) | 0.0363 (9) | |
N3 | 0.6541 (3) | 0.1013 (3) | 1.01155 (18) | 0.0431 (9) | |
N4 | 0.6879 (3) | −0.1346 (3) | 0.98703 (19) | 0.0451 (9) | |
N2 | 0.5349 (3) | 0.1544 (3) | 0.74323 (17) | 0.0380 (8) | |
C6 | 0.7111 (4) | −0.0898 (4) | 1.0577 (2) | 0.0437 (11) | |
C4 | 0.6252 (4) | −0.1065 (3) | 0.8530 (2) | 0.0367 (10) | |
C18 | 0.5825 (3) | −0.0328 (3) | 0.7924 (2) | 0.0326 (9) | |
C12 | 0.6338 (3) | 0.0564 (3) | 0.9431 (2) | 0.0368 (9) | |
C10 | 0.7204 (4) | 0.0719 (4) | 1.1443 (2) | 0.0578 (13) | |
H10A | 0.7108 | 0.1493 | 1.1527 | 0.069* | |
C13 | 0.5971 (4) | 0.1338 (3) | 0.8784 (2) | 0.0373 (10) | |
C17 | 0.5705 (3) | 0.0889 (3) | 0.8059 (2) | 0.0337 (9) | |
C19 | 0.2598 (4) | 0.0287 (4) | 0.5870 (2) | 0.0401 (10) | |
C11 | 0.6939 (4) | 0.0280 (4) | 1.0695 (2) | 0.0447 (11) | |
C1 | 0.5651 (4) | −0.1773 (3) | 0.7058 (2) | 0.0471 (11) | |
H1B | 0.5425 | −0.2025 | 0.6562 | 0.057* | |
C3 | 0.6421 (4) | −0.2206 (4) | 0.8354 (2) | 0.0489 (11) | |
H3B | 0.6739 | −0.2724 | 0.8734 | 0.059* | |
C14 | 0.5886 (4) | 0.2511 (4) | 0.8866 (2) | 0.0520 (12) | |
H14A | 0.6084 | 0.2842 | 0.9342 | 0.062* | |
C8 | 0.7748 (4) | −0.1170 (5) | 1.1915 (3) | 0.0652 (15) | |
H8A | 0.8001 | −0.1649 | 1.2327 | 0.078* | |
C2 | 0.6120 (4) | −0.2560 (4) | 0.7623 (2) | 0.0564 (13) | |
H2B | 0.6225 | −0.3319 | 0.7502 | 0.068* | |
C16 | 0.5236 (4) | 0.2654 (3) | 0.7536 (2) | 0.0490 (12) | |
H16A | 0.4958 | 0.3109 | 0.7115 | 0.059* | |
C9 | 0.7600 (4) | 0.0000 (5) | 1.2033 (3) | 0.0633 (14) | |
H9A | 0.7773 | 0.0288 | 1.2522 | 0.076* | |
C7 | 0.7525 (4) | −0.1619 (4) | 1.1197 (2) | 0.0551 (12) | |
H7A | 0.7647 | −0.2392 | 1.1124 | 0.066* | |
C15 | 0.5509 (5) | 0.3175 (4) | 0.8239 (2) | 0.0578 (13) | |
H15A | 0.5436 | 0.3960 | 0.8283 | 0.069* | |
O4 | 0.5077 (3) | 0.2196 (2) | 0.58662 (15) | 0.0508 (8) | |
O5 | 0.3983 (3) | 0.2030 (2) | 0.46817 (16) | 0.0588 (9) | |
C27 | 0.4606 (4) | 0.2578 (3) | 0.5222 (2) | 0.0405 (10) | |
C30 | 0.5377 (4) | 0.4530 (3) | 0.5701 (2) | 0.0384 (10) | |
C29 | 0.4429 (4) | 0.4323 (4) | 0.4403 (2) | 0.0388 (10) | |
C28 | 0.4816 (4) | 0.3832 (3) | 0.5108 (2) | 0.0344 (9) | |
C21 | 0.0943 (4) | −0.0796 (4) | 0.4949 (2) | 0.0406 (10) | |
C20 | 0.1242 (4) | 0.0122 (3) | 0.5429 (2) | 0.0342 (9) | |
C22 | 0.0299 (4) | 0.0927 (4) | 0.5484 (2) | 0.0408 (11) | |
H30 | 0.565 (3) | 0.424 (3) | 0.613 (2) | 0.040 (12)* | |
H22 | 0.049 (3) | 0.156 (3) | 0.5768 (19) | 0.036 (11)* | |
H21 | 0.161 (3) | −0.133 (3) | 0.4907 (18) | 0.033 (10)* | |
H3WA | 0.631 (4) | 0.045 (4) | 0.534 (3) | 0.075 (16)* | |
H3WB | 0.628 (5) | −0.048 (4) | 0.568 (3) | 0.08 (2)* | |
H29 | 0.404 (4) | 0.391 (3) | 0.401 (2) | 0.051 (13)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0429 (3) | 0.0306 (3) | 0.0290 (3) | −0.0023 (3) | 0.0033 (2) | 0.0023 (3) |
O1 | 0.0375 (17) | 0.0438 (17) | 0.0486 (18) | 0.0018 (14) | 0.0032 (14) | 0.0048 (14) |
O2 | 0.0464 (19) | 0.059 (2) | 0.0369 (17) | −0.0066 (15) | −0.0003 (14) | −0.0121 (15) |
O3 | 0.056 (2) | 0.037 (2) | 0.045 (2) | −0.0058 (16) | 0.0153 (16) | −0.0020 (17) |
N1 | 0.049 (2) | 0.0328 (18) | 0.0278 (18) | −0.0049 (17) | 0.0053 (15) | −0.0004 (16) |
C5 | 0.032 (2) | 0.047 (2) | 0.029 (2) | −0.003 (2) | 0.0049 (17) | 0.009 (2) |
N3 | 0.041 (2) | 0.059 (2) | 0.030 (2) | −0.0001 (17) | 0.0070 (16) | 0.0010 (17) |
N4 | 0.042 (2) | 0.057 (2) | 0.035 (2) | −0.0023 (17) | 0.0052 (17) | 0.0077 (18) |
N2 | 0.042 (2) | 0.036 (2) | 0.034 (2) | 0.0000 (16) | 0.0029 (16) | 0.0030 (16) |
C6 | 0.037 (2) | 0.063 (3) | 0.031 (2) | −0.004 (2) | 0.0061 (19) | 0.010 (2) |
C4 | 0.036 (2) | 0.037 (2) | 0.038 (2) | −0.0012 (18) | 0.0081 (19) | 0.0047 (19) |
C18 | 0.033 (2) | 0.031 (2) | 0.033 (2) | −0.0046 (17) | 0.0043 (18) | 0.0020 (17) |
C12 | 0.034 (2) | 0.049 (3) | 0.027 (2) | −0.002 (2) | 0.0035 (17) | 0.004 (2) |
C10 | 0.054 (3) | 0.084 (4) | 0.035 (3) | −0.002 (3) | 0.009 (2) | −0.001 (3) |
C13 | 0.038 (3) | 0.043 (3) | 0.030 (2) | −0.0001 (19) | 0.0029 (19) | 0.0008 (18) |
C17 | 0.032 (2) | 0.039 (2) | 0.029 (2) | −0.0021 (18) | 0.0024 (17) | 0.0018 (18) |
C19 | 0.044 (3) | 0.046 (3) | 0.030 (2) | −0.008 (2) | 0.007 (2) | 0.013 (2) |
C11 | 0.033 (2) | 0.070 (3) | 0.030 (2) | −0.002 (2) | 0.0035 (19) | 0.002 (2) |
C1 | 0.071 (3) | 0.035 (3) | 0.034 (2) | 0.000 (2) | 0.009 (2) | −0.003 (2) |
C3 | 0.063 (3) | 0.039 (3) | 0.043 (3) | 0.003 (2) | 0.008 (2) | 0.013 (2) |
C14 | 0.066 (3) | 0.048 (3) | 0.039 (3) | 0.001 (2) | 0.003 (2) | −0.008 (2) |
C8 | 0.060 (3) | 0.093 (4) | 0.038 (3) | −0.006 (3) | 0.000 (2) | 0.021 (3) |
C2 | 0.096 (4) | 0.031 (2) | 0.040 (3) | 0.001 (2) | 0.007 (3) | 0.004 (2) |
C16 | 0.068 (3) | 0.036 (3) | 0.041 (3) | 0.003 (2) | 0.006 (2) | 0.005 (2) |
C9 | 0.061 (3) | 0.092 (4) | 0.034 (3) | −0.011 (3) | 0.006 (2) | 0.001 (3) |
C7 | 0.053 (3) | 0.069 (3) | 0.040 (3) | −0.005 (2) | 0.001 (2) | 0.012 (2) |
C15 | 0.090 (4) | 0.032 (3) | 0.049 (3) | 0.006 (2) | 0.006 (3) | −0.004 (2) |
O4 | 0.075 (2) | 0.0348 (16) | 0.0403 (17) | −0.0023 (15) | 0.0061 (15) | 0.0125 (14) |
O5 | 0.096 (2) | 0.0325 (17) | 0.0463 (19) | −0.0056 (17) | 0.0109 (18) | −0.0029 (15) |
C27 | 0.050 (3) | 0.035 (2) | 0.041 (3) | 0.002 (2) | 0.019 (2) | 0.004 (2) |
C30 | 0.044 (3) | 0.036 (3) | 0.034 (2) | 0.003 (2) | 0.007 (2) | 0.012 (2) |
C29 | 0.047 (3) | 0.035 (2) | 0.035 (2) | −0.005 (2) | 0.007 (2) | 0.000 (2) |
C28 | 0.037 (2) | 0.030 (2) | 0.037 (2) | 0.0043 (18) | 0.0109 (19) | 0.0021 (18) |
C21 | 0.039 (3) | 0.040 (3) | 0.043 (2) | 0.004 (2) | 0.008 (2) | −0.003 (2) |
C20 | 0.037 (2) | 0.037 (2) | 0.028 (2) | −0.0051 (19) | 0.0049 (18) | 0.0017 (18) |
C22 | 0.044 (3) | 0.040 (3) | 0.038 (3) | −0.006 (2) | 0.006 (2) | −0.008 (2) |
Co1—O4 | 2.020 (3) | C19—C20 | 1.505 (5) |
Co1—O3 | 2.080 (3) | C1—C2 | 1.394 (5) |
Co1—O1 | 2.119 (3) | C1—H1B | 0.9300 |
Co1—N2 | 2.122 (3) | C3—C2 | 1.362 (5) |
Co1—N1 | 2.182 (3) | C3—H3B | 0.9300 |
Co1—O2 | 2.250 (3) | C14—C15 | 1.369 (5) |
Co1—C19 | 2.501 (4) | C14—H14A | 0.9300 |
O1—C19 | 1.275 (5) | C8—C7 | 1.377 (6) |
O2—C19 | 1.248 (5) | C8—C9 | 1.404 (7) |
O3—H3WA | 0.96 (5) | C8—H8A | 0.9300 |
O3—H3WB | 0.73 (5) | C2—H2B | 0.9300 |
N1—C1 | 1.335 (4) | C16—C15 | 1.389 (5) |
N1—C18 | 1.340 (4) | C16—H16A | 0.9300 |
C5—N4 | 1.336 (4) | C9—H9A | 0.9300 |
C5—C12 | 1.426 (5) | C7—H7A | 0.9300 |
C5—C4 | 1.462 (5) | C15—H15A | 0.9300 |
N3—C12 | 1.323 (5) | O4—C27 | 1.257 (4) |
N3—C11 | 1.358 (5) | O5—C27 | 1.243 (4) |
N4—C6 | 1.358 (5) | C27—C28 | 1.509 (5) |
N2—C16 | 1.325 (5) | C30—C29i | 1.381 (5) |
N2—C17 | 1.360 (4) | C30—C28 | 1.386 (5) |
C6—C7 | 1.404 (5) | C30—H30 | 0.85 (3) |
C6—C11 | 1.416 (6) | C29—C30i | 1.381 (5) |
C4—C3 | 1.397 (5) | C29—C28 | 1.386 (5) |
C4—C18 | 1.401 (5) | C29—H29 | 0.89 (4) |
C18—C17 | 1.460 (5) | C21—C20 | 1.380 (5) |
C12—C13 | 1.471 (5) | C21—C22ii | 1.394 (5) |
C10—C9 | 1.360 (6) | C21—H21 | 0.96 (3) |
C10—C11 | 1.422 (5) | C20—C22 | 1.389 (5) |
C10—H10A | 0.9300 | C22—C21ii | 1.394 (5) |
C13—C17 | 1.389 (5) | C22—H22 | 0.91 (3) |
C13—C14 | 1.390 (5) | ||
O4—Co1—O3 | 86.90 (14) | O2—C19—O1 | 120.9 (4) |
O4—Co1—O1 | 111.62 (10) | O2—C19—C20 | 120.2 (4) |
O3—Co1—O1 | 93.07 (12) | O1—C19—C20 | 118.9 (4) |
O4—Co1—N2 | 88.55 (12) | O2—C19—Co1 | 63.9 (2) |
O3—Co1—N2 | 123.37 (12) | O1—C19—Co1 | 57.9 (2) |
O1—Co1—N2 | 139.90 (12) | C20—C19—Co1 | 169.5 (3) |
O4—Co1—N1 | 156.75 (11) | N3—C11—C6 | 122.1 (4) |
O3—Co1—N1 | 87.56 (13) | N3—C11—C10 | 118.5 (4) |
O1—Co1—N1 | 91.21 (11) | C6—C11—C10 | 119.4 (4) |
N2—Co1—N1 | 75.79 (12) | N1—C1—C2 | 122.4 (4) |
O4—Co1—O2 | 88.58 (11) | N1—C1—H1B | 118.8 |
O3—Co1—O2 | 148.78 (12) | C2—C1—H1B | 118.8 |
O1—Co1—O2 | 60.22 (10) | C2—C3—C4 | 119.9 (4) |
N2—Co1—O2 | 87.34 (11) | C2—C3—H3B | 120.1 |
N1—Co1—O2 | 107.40 (11) | C4—C3—H3B | 120.1 |
O4—Co1—C19 | 98.53 (12) | C15—C14—C13 | 119.4 (4) |
O3—Co1—C19 | 120.97 (14) | C15—C14—H14A | 120.3 |
O1—Co1—C19 | 30.64 (11) | C13—C14—H14A | 120.3 |
N2—Co1—C19 | 115.53 (14) | C7—C8—C9 | 121.0 (5) |
N1—Co1—C19 | 103.67 (12) | C7—C8—H8A | 119.5 |
O2—Co1—C19 | 29.85 (11) | C9—C8—H8A | 119.5 |
C19—O1—Co1 | 91.5 (2) | C3—C2—C1 | 119.4 (4) |
C19—O2—Co1 | 86.3 (2) | C3—C2—H2B | 120.3 |
Co1—O3—H3WA | 112 (3) | C1—C2—H2B | 120.3 |
Co1—O3—H3WB | 115 (4) | N2—C16—C15 | 123.7 (4) |
H3WA—O3—H3WB | 95 (5) | N2—C16—H16A | 118.1 |
C1—N1—C18 | 117.8 (3) | C15—C16—H16A | 118.1 |
C1—N1—Co1 | 126.9 (3) | C10—C9—C8 | 120.9 (5) |
C18—N1—Co1 | 115.2 (2) | C10—C9—H9A | 119.6 |
N4—C5—C12 | 121.4 (4) | C8—C9—H9A | 119.6 |
N4—C5—C4 | 118.5 (4) | C8—C7—C6 | 119.4 (5) |
C12—C5—C4 | 120.1 (3) | C8—C7—H7A | 120.3 |
C12—N3—C11 | 116.0 (4) | C6—C7—H7A | 120.3 |
C5—N4—C6 | 116.7 (4) | C14—C15—C16 | 118.7 (4) |
C16—N2—C17 | 117.1 (3) | C14—C15—H15A | 120.6 |
C16—N2—Co1 | 125.9 (3) | C16—C15—H15A | 120.6 |
C17—N2—Co1 | 116.9 (2) | C27—O4—Co1 | 133.5 (3) |
N4—C6—C7 | 119.2 (4) | O5—C27—O4 | 126.5 (4) |
N4—C6—C11 | 121.0 (4) | O5—C27—C28 | 117.9 (4) |
C7—C6—C11 | 119.8 (4) | O4—C27—C28 | 115.6 (4) |
C3—C4—C18 | 116.7 (4) | C29i—C30—C28 | 121.5 (4) |
C3—C4—C5 | 123.6 (4) | C29i—C30—H30 | 119 (3) |
C18—C4—C5 | 119.6 (4) | C28—C30—H30 | 120 (3) |
N1—C18—C4 | 123.7 (3) | C30i—C29—C28 | 120.4 (4) |
N1—C18—C17 | 116.4 (3) | C30i—C29—H29 | 118 (3) |
C4—C18—C17 | 119.9 (3) | C28—C29—H29 | 121 (3) |
N3—C12—C5 | 122.7 (3) | C30—C28—C29 | 118.0 (4) |
N3—C12—C13 | 117.8 (4) | C30—C28—C27 | 121.6 (4) |
C5—C12—C13 | 119.5 (3) | C29—C28—C27 | 120.4 (4) |
C9—C10—C11 | 119.6 (5) | C20—C21—C22ii | 120.8 (4) |
C9—C10—H10A | 120.2 | C20—C21—H21 | 119 (2) |
C11—C10—H10A | 120.2 | C22ii—C21—H21 | 120 (2) |
C17—C13—C14 | 118.1 (4) | C21—C20—C22 | 119.9 (4) |
C17—C13—C12 | 119.2 (3) | C21—C20—C19 | 120.7 (4) |
C14—C13—C12 | 122.7 (4) | C22—C20—C19 | 119.4 (4) |
N2—C17—C13 | 122.9 (3) | C20—C22—C21ii | 119.3 (4) |
N2—C17—C18 | 115.6 (3) | C20—C22—H22 | 122 (2) |
C13—C17—C18 | 121.5 (3) | C21ii—C22—H22 | 119 (2) |
O4—Co1—O1—C19 | −69.1 (2) | Co1—O2—C19—O1 | 10.2 (4) |
O3—Co1—O1—C19 | −157.0 (2) | Co1—O2—C19—C20 | −169.0 (3) |
N2—Co1—O1—C19 | 46.2 (3) | Co1—O1—C19—O2 | −10.9 (4) |
N1—Co1—O1—C19 | 115.4 (2) | Co1—O1—C19—C20 | 168.4 (3) |
O2—Co1—O1—C19 | 5.9 (2) | O4—Co1—C19—O2 | −71.8 (2) |
O4—Co1—O2—C19 | 110.0 (2) | O3—Co1—C19—O2 | −163.3 (2) |
O3—Co1—O2—C19 | 28.3 (4) | O1—Co1—C19—O2 | 169.6 (4) |
O1—Co1—O2—C19 | −6.1 (2) | N2—Co1—C19—O2 | 20.6 (3) |
N2—Co1—O2—C19 | −161.4 (2) | N1—Co1—C19—O2 | 101.2 (2) |
N1—Co1—O2—C19 | −87.2 (2) | O4—Co1—C19—O1 | 118.6 (2) |
O4—Co1—N1—C1 | −127.2 (4) | O3—Co1—C19—O1 | 27.0 (3) |
O3—Co1—N1—C1 | −50.9 (3) | N2—Co1—C19—O1 | −149.0 (2) |
O1—Co1—N1—C1 | 42.2 (3) | N1—Co1—C19—O1 | −68.4 (2) |
N2—Co1—N1—C1 | −176.2 (3) | O2—Co1—C19—O1 | −169.6 (4) |
O2—Co1—N1—C1 | 101.2 (3) | O4—Co1—C19—C20 | 43.3 (18) |
C19—Co1—N1—C1 | 70.5 (4) | O3—Co1—C19—C20 | −48.2 (18) |
O4—Co1—N1—C18 | 49.1 (5) | O1—Co1—C19—C20 | −75.2 (17) |
O3—Co1—N1—C18 | 125.4 (3) | N2—Co1—C19—C20 | 135.8 (17) |
O1—Co1—N1—C18 | −141.6 (3) | N1—Co1—C19—C20 | −143.6 (17) |
N2—Co1—N1—C18 | 0.1 (3) | O2—Co1—C19—C20 | 115.2 (18) |
O2—Co1—N1—C18 | −82.5 (3) | C12—N3—C11—C6 | −0.8 (6) |
C19—Co1—N1—C18 | −113.3 (3) | C12—N3—C11—C10 | 178.4 (4) |
C12—C5—N4—C6 | −0.2 (5) | N4—C6—C11—N3 | −0.1 (6) |
C4—C5—N4—C6 | 179.3 (3) | C7—C6—C11—N3 | 180.0 (4) |
O4—Co1—N2—C16 | 18.7 (3) | N4—C6—C11—C10 | −179.4 (4) |
O3—Co1—N2—C16 | 104.0 (4) | C7—C6—C11—C10 | 0.7 (6) |
O1—Co1—N2—C16 | −104.1 (4) | C9—C10—C11—N3 | 179.7 (4) |
N1—Co1—N2—C16 | −178.6 (4) | C9—C10—C11—C6 | −1.0 (6) |
O2—Co1—N2—C16 | −69.9 (3) | C18—N1—C1—C2 | −1.2 (6) |
C19—Co1—N2—C16 | −80.0 (4) | Co1—N1—C1—C2 | 175.0 (3) |
O4—Co1—N2—C17 | −164.4 (3) | C18—C4—C3—C2 | −2.8 (6) |
O3—Co1—N2—C17 | −79.0 (3) | C5—C4—C3—C2 | 177.3 (4) |
O1—Co1—N2—C17 | 72.8 (3) | C17—C13—C14—C15 | 2.0 (6) |
N1—Co1—N2—C17 | −1.7 (3) | C12—C13—C14—C15 | −178.5 (4) |
O2—Co1—N2—C17 | 107.0 (3) | C4—C3—C2—C1 | 0.4 (7) |
C19—Co1—N2—C17 | 96.9 (3) | N1—C1—C2—C3 | 1.8 (7) |
C5—N4—C6—C7 | −179.5 (4) | C17—N2—C16—C15 | 2.7 (6) |
C5—N4—C6—C11 | 0.7 (6) | Co1—N2—C16—C15 | 179.6 (3) |
N4—C5—C4—C3 | −1.4 (6) | C11—C10—C9—C8 | 0.0 (7) |
C12—C5—C4—C3 | 178.1 (4) | C7—C8—C9—C10 | 1.4 (7) |
N4—C5—C4—C18 | 178.6 (3) | C9—C8—C7—C6 | −1.6 (7) |
C12—C5—C4—C18 | −1.9 (6) | N4—C6—C7—C8 | −179.3 (4) |
C1—N1—C18—C4 | −1.5 (6) | C11—C6—C7—C8 | 0.5 (6) |
Co1—N1—C18—C4 | −178.1 (3) | C13—C14—C15—C16 | −0.8 (7) |
C1—N1—C18—C17 | 178.1 (3) | N2—C16—C15—C14 | −1.7 (7) |
Co1—N1—C18—C17 | 1.5 (4) | O3—Co1—O4—C27 | 82.1 (4) |
C3—C4—C18—N1 | 3.4 (6) | O1—Co1—O4—C27 | −10.0 (4) |
C5—C4—C18—N1 | −176.6 (3) | N2—Co1—O4—C27 | −154.4 (4) |
C3—C4—C18—C17 | −176.1 (4) | N1—Co1—O4—C27 | 158.6 (4) |
C5—C4—C18—C17 | 3.9 (5) | O2—Co1—O4—C27 | −67.0 (4) |
C11—N3—C12—C5 | 1.3 (6) | C19—Co1—O4—C27 | −38.8 (4) |
C11—N3—C12—C13 | −176.9 (3) | Co1—O4—C27—O5 | −7.5 (7) |
N4—C5—C12—N3 | −0.8 (6) | Co1—O4—C27—C28 | 171.8 (3) |
C4—C5—C12—N3 | 179.7 (3) | C29i—C30—C28—C29 | −1.2 (7) |
N4—C5—C12—C13 | 177.4 (3) | C29i—C30—C28—C27 | 179.9 (4) |
C4—C5—C12—C13 | −2.1 (5) | C30i—C29—C28—C30 | 1.2 (7) |
N3—C12—C13—C17 | −177.7 (4) | C30i—C29—C28—C27 | −179.9 (4) |
C5—C12—C13—C17 | 4.1 (5) | O5—C27—C28—C30 | 173.0 (4) |
N3—C12—C13—C14 | 2.8 (6) | O4—C27—C28—C30 | −6.3 (6) |
C5—C12—C13—C14 | −175.4 (4) | O5—C27—C28—C29 | −5.9 (6) |
C16—N2—C17—C13 | −1.3 (6) | O4—C27—C28—C29 | 174.8 (4) |
Co1—N2—C17—C13 | −178.5 (3) | C22ii—C21—C20—C22 | 0.0 (7) |
C16—N2—C17—C18 | −179.8 (3) | C22ii—C21—C20—C19 | −177.4 (4) |
Co1—N2—C17—C18 | 3.0 (4) | O2—C19—C20—C21 | −173.8 (4) |
C14—C13—C17—N2 | −1.0 (6) | O1—C19—C20—C21 | 7.0 (5) |
C12—C13—C17—N2 | 179.5 (3) | Co1—C19—C20—C21 | 76.3 (18) |
C14—C13—C17—C18 | 177.4 (4) | O2—C19—C20—C22 | 8.8 (6) |
C12—C13—C17—C18 | −2.2 (6) | O1—C19—C20—C22 | −170.5 (4) |
N1—C18—C17—N2 | −2.9 (5) | Co1—C19—C20—C22 | −101.2 (18) |
C4—C18—C17—N2 | 176.6 (3) | C21—C20—C22—C21ii | 0.0 (7) |
N1—C18—C17—C13 | 178.6 (4) | C19—C20—C22—C21ii | 177.4 (4) |
C4—C18—C17—C13 | −1.9 (6) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3WA···O1iii | 0.96 (5) | 2.00 (5) | 2.877 (4) | 151 (4) |
O3—H3WB···O5iii | 0.73 (5) | 1.94 (5) | 2.666 (4) | 179 (6) |
Symmetry code: (iii) −x+1, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Co(C8H4O4)(C18H10N4)(H2O)] |
Mr | 523.36 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 292 |
a, b, c (Å) | 10.5218 (19), 11.742 (2), 18.077 (3) |
β (°) | 101.281 (4) |
V (Å3) | 2190.2 (7) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.83 |
Crystal size (mm) | 0.47 × 0.21 × 0.10 |
Data collection | |
Diffractometer | Bruker APEXII diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2002) |
Tmin, Tmax | 0.815, 0.924 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11590, 4317, 2417 |
Rint | 0.059 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.047, 0.114, 0.88 |
No. of reflections | 4317 |
No. of parameters | 349 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 1.70, −0.40 |
Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2002), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Sheldrick, 1990), SHELXTL-Plus.
Co1—O4 | 2.020 (3) | Co1—N2 | 2.122 (3) |
Co1—O3 | 2.080 (3) | Co1—N1 | 2.182 (3) |
Co1—O1 | 2.119 (3) | Co1—O2 | 2.250 (3) |
N2—Co1—N1 | 75.79 (12) | O1—Co1—O2 | 60.22 (10) |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3WA···O1i | 0.96 (5) | 2.00 (5) | 2.877 (4) | 151 (4) |
O3—H3WB···O5i | 0.73 (5) | 1.94 (5) | 2.666 (4) | 179 (6) |
Symmetry code: (i) −x+1, −y, −z+1. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register
1,10-Phenanthroline (phen) and its derivatives are important ligands with numerous uses in the constructon of metal-organic complexes. Supramolecular architectures based on the dipydo[3,2 - a:2',3'-c]phenazine (Dppz) molecule have considerably less attention (Li et al., 2006) As part of our ongoing studies in this area (Li et al., 2007), we now report the sythesis and structure of the title compound,(I), containing CoII ions, 1,4-BDC anions and phe-derived dipydo[3,2 - a:2',3'-c]phenazine (C18H10N4) ligands.
In compound (I), the CoII atom is six-coordinated by two N atoms from one Dppz molecule, three O atoms from two 1,4-BDC dianions (one monodentate, one bidentate) and one water molecule (Fig. 1, Table 1): a distorted octahedral cis-CoN2O4 arrangement is formed.
Neighboring CoII atoms are bridged by the centrosymmetric 1,4-BDC ligands forming a one-dimensional chain structure (Fig. 2). In the crystal structure, adjacent chains are connected through π-π interactions between dppz and 1,4-BDC ligands with a minimum centroid-centroid stacking distance of 3.459 (2) Å. O—H···O hydrogen bonds involving the water molecules and carboxylate O atom acceptors (Table 2) complete the structure of (I).