






Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807066032/bi2263sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536807066032/bi2263Isup2.hkl |
CCDC reference: 674349
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean
(C-C) = 0.002 Å
- R factor = 0.027
- wR factor = 0.071
- Data-to-parameter ratio = 14.8
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - O1 .. 5.06 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - O3 .. 5.33 su PLAT432_ALERT_2_C Short Inter X...Y Contact O11 .. C6 .. 2.99 Ang. PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 H2 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 5 H2 O
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
The proton-transfer compound, (tataH)2(pydc), was prepared by the reaction of pyridine-2,6-dicarboxylic acid (pydcH2) with 2,4,6-triamino-1,3,5-triazine (tata). The reaction between Co(NO3)2.6H2O (115 mg, 0.5 mmol) in water (20 ml) and (tataH)2(pydc) (420 mg, 1.0 mmol) in water (20 ml), in a 1:2 molar ratio gave a violet crystalline compound after slow evaporation of the solvent at room temperature.
The N-bound and O-bound H atoms were located in difference Fourier maps and their positions were freely refined. Other H atoms were placed in calculated positions (C—H = 0.93 Å) and refined as riding with Uiso(H) = 1.2Ueq(C).
Recently, we have reported the reactions between Co(NO3)2.6H2O and two proton-transfer compounds: (GH)2(pydc) (where G is guanidine) and (pipzH2)(pydc) (where pipz is piperazine) in a 1:2 molar ratio. These reactions lead to the formation of the complexes (GH)2[Co(H2O)6][Co(pydc)2]2 (Sheshmani et al., 2006) and (pipzH2)[Co(H2O)6][Co(pydc)2]2.8H2O (Aghabozorg, Attar Gharamaleki et al., 2007), respectively.
Here, we report the synthesis and X-ray crystal structure of the title compound (Fig. 1). The compound contains [Co(pydc)2]2- anions, [Co(H2O)6]2+ cations (site symmetry 1), and (tataH)+ cations. In the [Co(pydc)2]2- anions, the CoII atom is hexacoordinated by two N atoms (N1 and N2) and four O atoms (O1, O3, O5 and O7) from the carboxylate groups of two (pydc)2- groups that act as tridentate ligands. The coordination geometry is distorted octahedral, with atoms N1 and N2 occupying axial positions and the O atoms forming the equatorial plane. The N1—Co2—N2 angle deviates ca 7.7° from linearity. The mean Co—N and Co—O bond lengths for Co1 are 2.0214 (11) and 2.1658 (10) Å, respectively, consistent with similar complexes in the literature. The dihedral angle between the mean planes of the two (pydc)2- groups is 82.3 (1)°.
There is extensive O—H···O, N—H···O, N—H···N and C—H···O hydrogen bonding in the structure, as well as π–π stacking between (pydc)2- ligands with an interplanar distance of 3.484 (15) Å (symmetry operator: -x, -y + 1, -z + 1). Atom O8 of the C14?O8 carboxyl group lies above the N2/C9–C13 ring with an O···centroid distance of 3.240 (1) Å (symmetry operator: x, -y + 1, -z).
For related literature, see: Aghabozorg, Attar Gharamaleki, et al. (2007); Aghabozorg, Daneshvar, et al. (2007); Sheshmani et al. (2006).
Data collection: X-AREA (Stoe & Cie, 2005); cell refinement: X-AREA (Stoe & Cie, 2005); data reduction: X-RED32 (Stoe & Cie, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
(C3H7N6)2[Co(H2O)6][Co(C7H3NO4)2]2·4H2O | Z = 1 |
Mr = 1271.66 | F(000) = 651 |
Triclinic, P1 | Dx = 1.781 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.4003 (6) Å | Cell parameters from 2500 reflections |
b = 11.3014 (7) Å | θ = 1.9–29.2° |
c = 13.8794 (10) Å | µ = 1.15 mm−1 |
α = 95.901 (6)° | T = 120 K |
β = 106.017 (5)° | Block, violet |
γ = 107.133 (5)° | 0.50 × 0.50 × 0.45 mm |
V = 1185.73 (14) Å3 |
Stoe IPDSII diffractometer | 6289 independent reflections |
Radiation source: fine-focus sealed tube | 6111 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
φ scans | θmax = 29.2°, θmin = 1.9° |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 2004) | h = −11→11 |
Tmin = 0.570, Tmax = 0.595 | k = −15→15 |
14236 measured reflections | l = −18→18 |
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)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.071 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0323P)2 + 1.0178P] where P = (Fo2 + 2Fc2)/3 |
6289 reflections | (Δ/σ)max = 0.019 |
426 parameters | Δρmax = 0.48 e Å−3 |
0 restraints | Δρmin = −0.89 e Å−3 |
(C3H7N6)2[Co(H2O)6][Co(C7H3NO4)2]2·4H2O | γ = 107.133 (5)° |
Mr = 1271.66 | V = 1185.73 (14) Å3 |
Triclinic, P1 | Z = 1 |
a = 8.4003 (6) Å | Mo Kα radiation |
b = 11.3014 (7) Å | µ = 1.15 mm−1 |
c = 13.8794 (10) Å | T = 120 K |
α = 95.901 (6)° | 0.50 × 0.50 × 0.45 mm |
β = 106.017 (5)° |
Stoe IPDSII diffractometer | 6289 independent reflections |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 2004) | 6111 reflections with I > 2σ(I) |
Tmin = 0.570, Tmax = 0.595 | Rint = 0.021 |
14236 measured reflections |
R[F2 > 2σ(F2)] = 0.027 | 0 restraints |
wR(F2) = 0.071 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | Δρmax = 0.48 e Å−3 |
6289 reflections | Δρmin = −0.89 e Å−3 |
426 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 | ||
C1 | 0.09807 (17) | 0.59767 (12) | 0.39201 (10) | 0.0120 (2) | |
C2 | 0.19794 (16) | 0.52881 (12) | 0.46046 (9) | 0.0100 (2) | |
C3 | 0.26752 (17) | 0.56041 (12) | 0.56675 (10) | 0.0120 (2) | |
H3A | 0.2520 | 0.6273 | 0.6035 | 0.014* | |
C4 | 0.36138 (17) | 0.48851 (12) | 0.61643 (10) | 0.0123 (2) | |
H4 | 0.4087 | 0.5068 | 0.6874 | 0.015* | |
C5 | 0.38413 (17) | 0.38926 (12) | 0.55950 (10) | 0.0110 (2) | |
H5A | 0.4481 | 0.3416 | 0.5917 | 0.013* | |
C6 | 0.30917 (16) | 0.36313 (11) | 0.45369 (9) | 0.0092 (2) | |
C7 | 0.32416 (16) | 0.26121 (11) | 0.37973 (10) | 0.0099 (2) | |
C8 | −0.23329 (17) | 0.17773 (12) | 0.16471 (10) | 0.0110 (2) | |
C9 | −0.17660 (16) | 0.21879 (12) | 0.07477 (10) | 0.0102 (2) | |
C10 | −0.26571 (17) | 0.16132 (12) | −0.02722 (10) | 0.0118 (2) | |
H10A | −0.3694 | 0.0926 | −0.0460 | 0.014* | |
C11 | −0.19517 (17) | 0.20971 (12) | −0.10097 (10) | 0.0125 (2) | |
H11A | −0.2524 | 0.1736 | −0.1700 | 0.015* | |
C12 | −0.03839 (17) | 0.31260 (12) | −0.07062 (10) | 0.0118 (2) | |
H12A | 0.0096 | 0.3464 | −0.1188 | 0.014* | |
C13 | 0.04411 (16) | 0.36325 (11) | 0.03343 (9) | 0.0096 (2) | |
C14 | 0.21779 (16) | 0.47113 (12) | 0.08186 (10) | 0.0102 (2) | |
C15 | 0.34004 (16) | 0.22483 (12) | 0.01662 (10) | 0.0102 (2) | |
C16 | 0.12106 (17) | 0.07415 (12) | −0.11206 (10) | 0.0112 (2) | |
C17 | 0.33515 (17) | 0.21334 (12) | −0.15514 (10) | 0.0111 (2) | |
N1 | 0.21838 (14) | 0.43202 (10) | 0.40734 (8) | 0.00895 (19) | |
N2 | −0.02564 (14) | 0.31650 (10) | 0.10290 (8) | 0.00952 (19) | |
N3 | 0.41635 (16) | 0.28384 (11) | 0.11324 (9) | 0.0126 (2) | |
H3B | 0.504 (3) | 0.349 (2) | 0.1304 (17) | 0.027 (5)* | |
H3C | 0.370 (3) | 0.258 (2) | 0.1568 (17) | 0.021 (5)* | |
N4 | 0.19481 (15) | 0.12353 (10) | −0.01054 (8) | 0.0114 (2) | |
N5 | −0.02803 (16) | −0.02294 (11) | −0.14102 (9) | 0.0145 (2) | |
H5B | −0.079 (3) | −0.057 (2) | −0.2023 (19) | 0.029 (6)* | |
H5C | −0.073 (3) | −0.049 (2) | −0.0984 (18) | 0.025 (5)* | |
N6 | 0.18535 (15) | 0.11571 (11) | −0.18643 (8) | 0.0118 (2) | |
N7 | 0.41327 (17) | 0.25597 (11) | −0.22155 (9) | 0.0142 (2) | |
H7A | 0.369 (3) | 0.218 (2) | −0.2810 (17) | 0.022 (5)* | |
H7B | 0.497 (3) | 0.320 (2) | −0.2040 (17) | 0.022 (5)* | |
N8 | 0.41245 (15) | 0.27160 (11) | −0.05467 (8) | 0.0113 (2) | |
H8 | 0.504 (3) | 0.337 (2) | −0.0403 (19) | 0.034 (6)* | |
O1 | 0.04288 (13) | 0.54960 (9) | 0.29686 (7) | 0.01419 (18) | |
O2 | 0.07887 (16) | 0.69381 (10) | 0.43161 (8) | 0.0199 (2) | |
O3 | 0.26322 (13) | 0.26350 (9) | 0.28504 (7) | 0.01189 (17) | |
O4 | 0.39502 (13) | 0.18586 (9) | 0.41537 (8) | 0.01399 (18) | |
O5 | −0.12884 (13) | 0.24112 (9) | 0.25325 (7) | 0.01391 (18) | |
O6 | −0.37131 (13) | 0.08811 (10) | 0.14719 (8) | 0.01572 (19) | |
O7 | 0.27238 (12) | 0.50218 (9) | 0.17825 (7) | 0.01198 (17) | |
O8 | 0.29441 (13) | 0.52186 (9) | 0.02292 (7) | 0.01449 (18) | |
O9 | 0.04230 (14) | −0.08822 (10) | 0.37722 (8) | 0.01480 (19) | |
H9A | −0.024 (4) | −0.097 (3) | 0.322 (2) | 0.043 (7)* | |
H9B | 0.053 (3) | −0.162 (3) | 0.381 (2) | 0.043 (7)* | |
O10 | −0.27658 (13) | −0.08879 (9) | 0.43229 (8) | 0.01282 (18) | |
H10B | −0.331 (3) | −0.047 (2) | 0.404 (2) | 0.035 (6)* | |
H10C | −0.321 (3) | −0.116 (2) | 0.4736 (19) | 0.032 (6)* | |
O11 | −0.02330 (13) | 0.15266 (9) | 0.42733 (8) | 0.01306 (18) | |
H11B | −0.071 (3) | 0.158 (2) | 0.370 (2) | 0.033 (6)* | |
H11C | −0.044 (3) | 0.207 (2) | 0.4624 (18) | 0.028 (6)* | |
O12 | −0.47942 (15) | 0.01920 (11) | 0.31460 (9) | 0.0196 (2) | |
H12B | −0.512 (3) | 0.069 (2) | 0.340 (2) | 0.036 (6)* | |
H12C | −0.443 (3) | 0.048 (2) | 0.268 (2) | 0.033 (6)* | |
O13 | 0.29453 (14) | 0.49240 (11) | −0.16999 (8) | 0.0180 (2) | |
H13A | 0.205 (4) | 0.480 (2) | −0.210 (2) | 0.039 (7)* | |
H13B | 0.277 (3) | 0.488 (2) | −0.115 (2) | 0.037 (6)* | |
Co1 | 0.10510 (2) | 0.385862 (16) | 0.253625 (12) | 0.00886 (5) | |
Co2 | 0.0000 | 0.0000 | 0.5000 | 0.01165 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0127 (5) | 0.0121 (5) | 0.0124 (6) | 0.0050 (4) | 0.0048 (4) | 0.0029 (4) |
C2 | 0.0104 (5) | 0.0095 (5) | 0.0101 (5) | 0.0027 (4) | 0.0042 (4) | 0.0016 (4) |
C3 | 0.0132 (5) | 0.0119 (5) | 0.0100 (5) | 0.0032 (4) | 0.0047 (4) | −0.0005 (4) |
C4 | 0.0133 (5) | 0.0131 (5) | 0.0086 (5) | 0.0016 (4) | 0.0039 (4) | 0.0011 (4) |
C5 | 0.0112 (5) | 0.0108 (5) | 0.0101 (5) | 0.0022 (4) | 0.0032 (4) | 0.0037 (4) |
C6 | 0.0094 (5) | 0.0083 (5) | 0.0096 (5) | 0.0019 (4) | 0.0039 (4) | 0.0018 (4) |
C7 | 0.0100 (5) | 0.0087 (5) | 0.0111 (5) | 0.0019 (4) | 0.0049 (4) | 0.0017 (4) |
C8 | 0.0118 (5) | 0.0109 (5) | 0.0111 (5) | 0.0045 (4) | 0.0037 (4) | 0.0034 (4) |
C9 | 0.0107 (5) | 0.0094 (5) | 0.0108 (5) | 0.0036 (4) | 0.0034 (4) | 0.0023 (4) |
C10 | 0.0110 (5) | 0.0107 (5) | 0.0120 (6) | 0.0029 (4) | 0.0019 (4) | 0.0015 (4) |
C11 | 0.0137 (6) | 0.0137 (6) | 0.0082 (5) | 0.0046 (5) | 0.0012 (4) | 0.0001 (4) |
C12 | 0.0133 (6) | 0.0131 (6) | 0.0089 (5) | 0.0044 (5) | 0.0035 (4) | 0.0022 (4) |
C13 | 0.0104 (5) | 0.0092 (5) | 0.0092 (5) | 0.0034 (4) | 0.0029 (4) | 0.0018 (4) |
C14 | 0.0108 (5) | 0.0087 (5) | 0.0108 (5) | 0.0032 (4) | 0.0036 (4) | 0.0015 (4) |
C15 | 0.0116 (5) | 0.0102 (5) | 0.0104 (5) | 0.0055 (4) | 0.0040 (4) | 0.0024 (4) |
C16 | 0.0129 (5) | 0.0092 (5) | 0.0118 (6) | 0.0045 (4) | 0.0036 (4) | 0.0020 (4) |
C17 | 0.0132 (5) | 0.0107 (5) | 0.0103 (5) | 0.0054 (4) | 0.0039 (4) | 0.0018 (4) |
N1 | 0.0094 (4) | 0.0086 (4) | 0.0083 (4) | 0.0019 (4) | 0.0032 (4) | 0.0015 (4) |
N2 | 0.0105 (5) | 0.0094 (4) | 0.0084 (4) | 0.0034 (4) | 0.0026 (4) | 0.0017 (4) |
N3 | 0.0137 (5) | 0.0129 (5) | 0.0095 (5) | 0.0021 (4) | 0.0039 (4) | 0.0012 (4) |
N4 | 0.0123 (5) | 0.0107 (5) | 0.0098 (5) | 0.0024 (4) | 0.0032 (4) | 0.0015 (4) |
N5 | 0.0147 (5) | 0.0131 (5) | 0.0115 (5) | −0.0002 (4) | 0.0039 (4) | 0.0000 (4) |
N6 | 0.0131 (5) | 0.0113 (5) | 0.0094 (5) | 0.0025 (4) | 0.0032 (4) | 0.0014 (4) |
N7 | 0.0169 (5) | 0.0126 (5) | 0.0103 (5) | 0.0003 (4) | 0.0059 (4) | 0.0005 (4) |
N8 | 0.0115 (5) | 0.0113 (5) | 0.0092 (5) | 0.0013 (4) | 0.0038 (4) | 0.0008 (4) |
O1 | 0.0176 (5) | 0.0155 (4) | 0.0107 (4) | 0.0089 (4) | 0.0033 (4) | 0.0020 (3) |
O2 | 0.0300 (6) | 0.0169 (5) | 0.0167 (5) | 0.0149 (4) | 0.0067 (4) | 0.0016 (4) |
O3 | 0.0142 (4) | 0.0128 (4) | 0.0088 (4) | 0.0053 (3) | 0.0035 (3) | 0.0011 (3) |
O4 | 0.0184 (5) | 0.0137 (4) | 0.0146 (4) | 0.0089 (4) | 0.0078 (4) | 0.0057 (3) |
O5 | 0.0141 (4) | 0.0150 (4) | 0.0096 (4) | 0.0009 (4) | 0.0034 (3) | 0.0028 (3) |
O6 | 0.0131 (4) | 0.0149 (4) | 0.0155 (4) | −0.0006 (4) | 0.0049 (4) | 0.0029 (4) |
O7 | 0.0126 (4) | 0.0122 (4) | 0.0092 (4) | 0.0018 (3) | 0.0033 (3) | 0.0015 (3) |
O8 | 0.0157 (4) | 0.0147 (4) | 0.0110 (4) | 0.0005 (4) | 0.0061 (4) | 0.0026 (3) |
O9 | 0.0201 (5) | 0.0161 (5) | 0.0092 (4) | 0.0093 (4) | 0.0034 (4) | 0.0011 (4) |
O10 | 0.0156 (4) | 0.0126 (4) | 0.0115 (4) | 0.0053 (4) | 0.0050 (4) | 0.0044 (3) |
O11 | 0.0183 (5) | 0.0114 (4) | 0.0108 (4) | 0.0066 (4) | 0.0045 (4) | 0.0036 (3) |
O12 | 0.0271 (6) | 0.0227 (5) | 0.0190 (5) | 0.0157 (5) | 0.0131 (4) | 0.0095 (4) |
O13 | 0.0139 (5) | 0.0264 (5) | 0.0110 (4) | 0.0030 (4) | 0.0041 (4) | 0.0031 (4) |
Co1 | 0.01010 (9) | 0.00890 (8) | 0.00667 (8) | 0.00262 (6) | 0.00218 (6) | 0.00084 (6) |
Co2 | 0.01542 (12) | 0.01014 (11) | 0.00968 (11) | 0.00476 (9) | 0.00401 (9) | 0.00194 (8) |
C1—O2 | 1.2401 (16) | C16—N4 | 1.3541 (16) |
C1—O1 | 1.2729 (16) | C16—N6 | 1.3548 (16) |
C1—C2 | 1.5195 (17) | C17—N7 | 1.3232 (17) |
C2—N1 | 1.3358 (16) | C17—N6 | 1.3310 (17) |
C2—C3 | 1.3922 (17) | C17—N8 | 1.3636 (16) |
C3—C4 | 1.3965 (18) | N1—Co1 | 2.0218 (11) |
C3—H3A | 0.930 | N2—Co1 | 2.0211 (11) |
C4—C5 | 1.3952 (18) | N3—H3B | 0.83 (2) |
C4—H4 | 0.930 | N3—H3C | 0.84 (2) |
C5—C6 | 1.3898 (17) | N5—H5B | 0.83 (2) |
C5—H5A | 0.930 | N5—H5C | 0.82 (2) |
C6—N1 | 1.3356 (16) | N7—H7A | 0.82 (2) |
C6—C7 | 1.5199 (17) | N7—H7B | 0.81 (2) |
C7—O4 | 1.2438 (16) | N8—H8 | 0.86 (3) |
C7—O3 | 1.2781 (15) | O1—Co1 | 2.1383 (10) |
C8—O6 | 1.2373 (16) | O3—Co1 | 2.1802 (10) |
C8—O5 | 1.2833 (16) | O5—Co1 | 2.1532 (10) |
C8—C9 | 1.5223 (17) | O7—Co1 | 2.1916 (9) |
C9—N2 | 1.3391 (16) | O9—Co2 | 2.0538 (10) |
C9—C10 | 1.3877 (17) | O9—H9A | 0.79 (3) |
C10—C11 | 1.3989 (18) | O9—H9B | 0.87 (3) |
C10—H10A | 0.930 | O10—Co2 | 2.1250 (10) |
C11—C12 | 1.3982 (18) | O10—H10B | 0.81 (3) |
C11—H11A | 0.930 | O10—H10C | 0.81 (3) |
C12—C13 | 1.3920 (17) | O11—Co2 | 2.1166 (10) |
C12—H12A | 0.930 | O11—H11B | 0.81 (3) |
C13—N2 | 1.3364 (16) | O11—H11C | 0.83 (3) |
C13—C14 | 1.5196 (17) | O12—H12B | 0.79 (3) |
C14—O8 | 1.2576 (15) | O12—H12C | 0.85 (3) |
C14—O7 | 1.2624 (15) | O13—H13A | 0.77 (3) |
C15—N3 | 1.3205 (17) | O13—H13B | 0.83 (3) |
C15—N4 | 1.3324 (16) | Co2—O9i | 2.0538 (10) |
C15—N8 | 1.3706 (16) | Co2—O11i | 2.1166 (10) |
C16—N5 | 1.3251 (17) | Co2—O10i | 2.1250 (10) |
O2—C1—O1 | 126.05 (12) | C15—N3—H3C | 118.9 (14) |
O2—C1—C2 | 118.92 (12) | H3B—N3—H3C | 120 (2) |
O1—C1—C2 | 115.03 (11) | C15—N4—C16 | 115.97 (11) |
N1—C2—C3 | 121.29 (12) | C16—N5—H5B | 121.4 (16) |
N1—C2—C1 | 112.54 (11) | C16—N5—H5C | 120.0 (16) |
C3—C2—C1 | 126.15 (11) | H5B—N5—H5C | 119 (2) |
C2—C3—C4 | 117.93 (12) | C17—N6—C16 | 115.98 (11) |
C2—C3—H3A | 121.0 | C17—N7—H7A | 117.6 (15) |
C4—C3—H3A | 121.0 | C17—N7—H7B | 120.4 (15) |
C5—C4—C3 | 119.94 (12) | H7A—N7—H7B | 122 (2) |
C5—C4—H4 | 120.0 | C17—N8—C15 | 119.54 (11) |
C3—C4—H4 | 120.0 | C17—N8—H8 | 116.7 (16) |
C6—C5—C4 | 118.55 (12) | C15—N8—H8 | 123.8 (16) |
C6—C5—H5A | 120.7 | C1—O1—Co1 | 116.52 (8) |
C4—C5—H5A | 120.7 | C7—O3—Co1 | 114.43 (8) |
N1—C6—C5 | 120.80 (11) | C8—O5—Co1 | 115.52 (8) |
N1—C6—C7 | 113.45 (11) | C14—O7—Co1 | 114.48 (8) |
C5—C6—C7 | 125.72 (11) | Co2—O9—H9A | 119 (2) |
O4—C7—O3 | 126.28 (12) | Co2—O9—H9B | 116.3 (18) |
O4—C7—C6 | 118.49 (11) | H9A—O9—H9B | 105 (3) |
O3—C7—C6 | 115.22 (11) | Co2—O10—H10B | 117.2 (18) |
O6—C8—O5 | 126.18 (12) | Co2—O10—H10C | 111.2 (17) |
O6—C8—C9 | 118.67 (11) | H10B—O10—H10C | 107 (2) |
O5—C8—C9 | 115.14 (11) | Co2—O11—H11B | 134.2 (18) |
N2—C9—C10 | 121.47 (12) | Co2—O11—H11C | 113.0 (16) |
N2—C9—C8 | 113.40 (11) | H11B—O11—H11C | 102 (2) |
C10—C9—C8 | 125.11 (11) | H12B—O12—H12C | 108 (2) |
C9—C10—C11 | 118.14 (12) | H13A—O13—H13B | 107 (3) |
C9—C10—H10A | 120.9 | N2—Co1—N1 | 172.24 (4) |
C11—C10—H10A | 120.9 | N2—Co1—O1 | 107.89 (4) |
C12—C11—C10 | 119.79 (12) | N1—Co1—O1 | 76.33 (4) |
C12—C11—H11A | 120.1 | N2—Co1—O5 | 76.99 (4) |
C10—C11—H11A | 120.1 | N1—Co1—O5 | 96.02 (4) |
C13—C12—C11 | 118.36 (12) | O1—Co1—O5 | 99.47 (4) |
C13—C12—H12A | 120.8 | N2—Co1—O3 | 100.34 (4) |
C11—C12—H12A | 120.8 | N1—Co1—O3 | 76.35 (4) |
N2—C13—C12 | 121.12 (11) | O1—Co1—O3 | 151.15 (4) |
N2—C13—C14 | 112.50 (11) | O5—Co1—O3 | 92.44 (4) |
C12—C13—C14 | 126.37 (11) | N2—Co1—O7 | 76.19 (4) |
O8—C14—O7 | 125.66 (12) | N1—Co1—O7 | 110.86 (4) |
O8—C14—C13 | 117.54 (11) | O1—Co1—O7 | 87.05 (4) |
O7—C14—C13 | 116.80 (11) | O5—Co1—O7 | 153.11 (4) |
N3—C15—N4 | 120.51 (12) | O3—Co1—O7 | 94.11 (4) |
N3—C15—N8 | 118.32 (12) | O9—Co2—O9i | 180.000 (1) |
N4—C15—N8 | 121.16 (11) | O9—Co2—O11i | 88.64 (4) |
N5—C16—N4 | 116.86 (12) | O9i—Co2—O11i | 91.36 (4) |
N5—C16—N6 | 117.28 (12) | O9—Co2—O11 | 91.36 (4) |
N4—C16—N6 | 125.86 (12) | O9i—Co2—O11 | 88.64 (4) |
N7—C17—N6 | 120.34 (12) | O11i—Co2—O11 | 180.0 |
N7—C17—N8 | 118.30 (12) | O9—Co2—O10i | 89.04 (4) |
N6—C17—N8 | 121.36 (12) | O9i—Co2—O10i | 90.96 (4) |
C6—N1—C2 | 121.47 (11) | O11i—Co2—O10i | 87.97 (4) |
C6—N1—Co1 | 119.06 (8) | O11—Co2—O10i | 92.03 (4) |
C2—N1—Co1 | 119.45 (9) | O9—Co2—O10 | 90.96 (4) |
C13—N2—C9 | 121.11 (11) | O9i—Co2—O10 | 89.04 (4) |
C13—N2—Co1 | 119.93 (9) | O11i—Co2—O10 | 92.03 (4) |
C9—N2—Co1 | 118.84 (9) | O11—Co2—O10 | 87.97 (4) |
C15—N3—H3B | 121.1 (16) | O10i—Co2—O10 | 180.00 (6) |
O2—C1—C2—N1 | −175.99 (12) | N5—C16—N6—C17 | 179.97 (12) |
O1—C1—C2—N1 | 3.28 (16) | N4—C16—N6—C17 | 0.49 (19) |
O2—C1—C2—C3 | 2.4 (2) | N7—C17—N8—C15 | −176.18 (12) |
O1—C1—C2—C3 | −178.33 (12) | N6—C17—N8—C15 | 3.55 (19) |
N1—C2—C3—C4 | 0.67 (19) | N3—C15—N8—C17 | −179.25 (12) |
C1—C2—C3—C4 | −177.60 (12) | N4—C15—N8—C17 | −0.25 (19) |
C2—C3—C4—C5 | 0.53 (19) | O2—C1—O1—Co1 | 178.25 (11) |
C3—C4—C5—C6 | −1.09 (18) | C2—C1—O1—Co1 | −0.95 (14) |
C4—C5—C6—N1 | 0.48 (18) | O4—C7—O3—Co1 | 168.69 (10) |
C4—C5—C6—C7 | 178.42 (11) | C6—C7—O3—Co1 | −12.44 (13) |
N1—C6—C7—O4 | −174.80 (11) | O6—C8—O5—Co1 | 177.49 (11) |
C5—C6—C7—O4 | 7.12 (19) | C9—C8—O5—Co1 | −1.93 (14) |
N1—C6—C7—O3 | 6.23 (15) | O8—C14—O7—Co1 | −177.89 (10) |
C5—C6—C7—O3 | −171.84 (12) | C13—C14—O7—Co1 | 2.28 (14) |
O6—C8—C9—N2 | 179.96 (12) | C13—N2—Co1—O1 | 84.95 (10) |
O5—C8—C9—N2 | −0.58 (16) | C9—N2—Co1—O1 | −99.00 (10) |
O6—C8—C9—C10 | −1.74 (19) | C13—N2—Co1—O5 | −179.15 (10) |
O5—C8—C9—C10 | 177.73 (12) | C9—N2—Co1—O5 | −3.10 (9) |
N2—C9—C10—C11 | −1.12 (19) | C13—N2—Co1—O3 | −89.02 (10) |
C8—C9—C10—C11 | −179.30 (12) | C9—N2—Co1—O3 | 87.03 (10) |
C9—C10—C11—C12 | 0.45 (19) | C13—N2—Co1—O7 | 2.71 (9) |
C10—C11—C12—C13 | 0.63 (19) | C9—N2—Co1—O7 | 178.76 (10) |
C11—C12—C13—N2 | −1.12 (19) | C6—N1—Co1—O1 | −178.41 (10) |
C11—C12—C13—C14 | 177.53 (12) | C2—N1—Co1—O1 | 2.95 (9) |
N2—C13—C14—O8 | −179.98 (11) | C6—N1—Co1—O5 | 83.28 (9) |
C12—C13—C14—O8 | 1.28 (19) | C2—N1—Co1—O5 | −95.36 (9) |
N2—C13—C14—O7 | −0.13 (16) | C6—N1—Co1—O3 | −7.78 (9) |
C12—C13—C14—O7 | −178.88 (12) | C2—N1—Co1—O3 | 173.58 (10) |
C5—C6—N1—C2 | 0.73 (18) | C6—N1—Co1—O7 | −97.00 (9) |
C7—C6—N1—C2 | −177.45 (11) | C2—N1—Co1—O7 | 84.36 (10) |
C5—C6—N1—Co1 | −177.89 (9) | C1—O1—Co1—N2 | 172.32 (9) |
C7—C6—N1—Co1 | 3.94 (14) | C1—O1—Co1—N1 | −0.91 (9) |
C3—C2—N1—C6 | −1.32 (18) | C1—O1—Co1—O5 | 93.04 (10) |
C1—C2—N1—C6 | 177.17 (11) | C1—O1—Co1—O3 | −20.05 (14) |
C3—C2—N1—Co1 | 177.29 (9) | C1—O1—Co1—O7 | −113.22 (10) |
C1—C2—N1—Co1 | −4.23 (14) | C8—O5—Co1—N2 | 2.70 (9) |
C12—C13—N2—C9 | 0.48 (19) | C8—O5—Co1—N1 | −173.89 (9) |
C14—C13—N2—C9 | −178.34 (11) | C8—O5—Co1—O1 | 109.02 (9) |
C12—C13—N2—Co1 | 176.44 (9) | C8—O5—Co1—O3 | −97.36 (9) |
C14—C13—N2—Co1 | −2.38 (14) | C8—O5—Co1—O7 | 6.70 (15) |
C10—C9—N2—C13 | 0.67 (19) | C7—O3—Co1—N2 | −161.61 (9) |
C8—C9—N2—C13 | 179.04 (11) | C7—O3—Co1—N1 | 11.20 (9) |
C10—C9—N2—Co1 | −175.33 (9) | C7—O3—Co1—O1 | 30.34 (13) |
C8—C9—N2—Co1 | 3.04 (14) | C7—O3—Co1—O5 | −84.40 (9) |
N3—C15—N4—C16 | 176.38 (12) | C7—O3—Co1—O7 | 121.69 (9) |
N8—C15—N4—C16 | −2.61 (18) | C14—O7—Co1—N2 | −2.67 (9) |
N5—C16—N4—C15 | −176.90 (12) | C14—O7—Co1—N1 | 173.94 (9) |
N6—C16—N4—C15 | 2.58 (19) | C14—O7—Co1—O1 | −111.90 (9) |
N7—C17—N6—C16 | 176.15 (12) | C14—O7—Co1—O5 | −6.68 (14) |
N8—C17—N6—C16 | −3.57 (18) | C14—O7—Co1—O3 | 96.99 (9) |
Symmetry code: (i) −x, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
N3—H3B···O13ii | 0.83 (2) | 1.97 (2) | 2.7982 (18) | 178 (3) |
N3—H3C···O3 | 0.84 (2) | 2.21 (2) | 3.0041 (17) | 159 (2) |
N5—H5B···O3iii | 0.83 (2) | 2.35 (2) | 2.9713 (16) | 133 (2) |
N5—H5C···N4iii | 0.82 (2) | 2.16 (2) | 2.9765 (17) | 178 (3) |
N7—H7A···O10iii | 0.82 (2) | 2.22 (2) | 3.0291 (16) | 169 (2) |
N7—H7B···O7ii | 0.80 (2) | 2.26 (2) | 3.0560 (17) | 172 (2) |
N8—H8···O8ii | 0.85 (2) | 1.89 (2) | 2.7404 (17) | 174 (2) |
O9—H9A···N6iii | 0.79 (3) | 1.94 (3) | 2.7298 (16) | 179 (4) |
O9—H9B···O2iv | 0.87 (3) | 1.89 (3) | 2.7263 (16) | 162 (3) |
O10—H10B···O12 | 0.81 (2) | 1.88 (3) | 2.6759 (17) | 167 (3) |
O10—H10C···O4i | 0.81 (2) | 1.97 (2) | 2.7675 (15) | 171 (3) |
O11—H11B···O5 | 0.80 (3) | 1.97 (2) | 2.7313 (14) | 157 (2) |
O11—H11C···O2v | 0.83 (2) | 1.90 (2) | 2.7101 (16) | 165 (2) |
O12—H12B···O4vi | 0.79 (3) | 2.06 (3) | 2.8389 (17) | 174 (2) |
O12—H12C···O6 | 0.84 (3) | 1.98 (3) | 2.8196 (16) | 171 (2) |
O13—H13A···O1vii | 0.77 (3) | 2.01 (3) | 2.7642 (16) | 171 (3) |
O13—H13B···O8 | 0.82 (3) | 1.87 (3) | 2.6642 (14) | 163 (2) |
C4—H4···O13viii | 0.93 | 2.43 | 3.164 (2) | 136 |
C10—H10A···O6ix | 0.93 | 2.45 | 3.344 (2) | 162 |
Symmetry codes: (i) −x, −y, −z+1; (ii) −x+1, −y+1, −z; (iii) −x, −y, −z; (iv) x, y−1, z; (v) −x, −y+1, −z+1; (vi) x−1, y, z; (vii) −x, −y+1, −z; (viii) x, y, z+1; (ix) −x−1, −y, −z. |
Experimental details
Crystal data | |
Chemical formula | (C3H7N6)2[Co(H2O)6][Co(C7H3NO4)2]2·4H2O |
Mr | 1271.66 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 120 |
a, b, c (Å) | 8.4003 (6), 11.3014 (7), 13.8794 (10) |
α, β, γ (°) | 95.901 (6), 106.017 (5), 107.133 (5) |
V (Å3) | 1185.73 (14) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.15 |
Crystal size (mm) | 0.50 × 0.50 × 0.45 |
Data collection | |
Diffractometer | Stoe IPDSII |
Absorption correction | Numerical (X-SHAPE; Stoe & Cie, 2004) |
Tmin, Tmax | 0.570, 0.595 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14236, 6289, 6111 |
Rint | 0.021 |
(sin θ/λ)max (Å−1) | 0.686 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.027, 0.071, 1.06 |
No. of reflections | 6289 |
No. of parameters | 426 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.48, −0.89 |
Computer programs: X-AREA (Stoe & Cie, 2005), X-RED32 (Stoe & Cie, 2005), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).
D—H···A | D—H | H···A | D···A | D—H···A |
N3—H3B···O13i | 0.83 (2) | 1.97 (2) | 2.7982 (18) | 178 (3) |
N3—H3C···O3 | 0.84 (2) | 2.21 (2) | 3.0041 (17) | 159 (2) |
N5—H5B···O3ii | 0.83 (2) | 2.35 (2) | 2.9713 (16) | 133 (2) |
N5—H5C···N4ii | 0.82 (2) | 2.16 (2) | 2.9765 (17) | 178 (3) |
N7—H7A···O10ii | 0.82 (2) | 2.22 (2) | 3.0291 (16) | 169 (2) |
N7—H7B···O7i | 0.80 (2) | 2.26 (2) | 3.0560 (17) | 172 (2) |
N8—H8···O8i | 0.85 (2) | 1.89 (2) | 2.7404 (17) | 174 (2) |
O9—H9A···N6ii | 0.79 (3) | 1.94 (3) | 2.7298 (16) | 179 (4) |
O9—H9B···O2iii | 0.87 (3) | 1.89 (3) | 2.7263 (16) | 162 (3) |
O10—H10B···O12 | 0.81 (2) | 1.88 (3) | 2.6759 (17) | 167 (3) |
O10—H10C···O4iv | 0.81 (2) | 1.97 (2) | 2.7675 (15) | 171 (3) |
O11—H11B···O5 | 0.80 (3) | 1.97 (2) | 2.7313 (14) | 157 (2) |
O11—H11C···O2v | 0.83 (2) | 1.90 (2) | 2.7101 (16) | 165 (2) |
O12—H12B···O4vi | 0.79 (3) | 2.06 (3) | 2.8389 (17) | 174 (2) |
O12—H12C···O6 | 0.84 (3) | 1.98 (3) | 2.8196 (16) | 171 (2) |
O13—H13A···O1vii | 0.77 (3) | 2.01 (3) | 2.7642 (16) | 171 (3) |
O13—H13B···O8 | 0.82 (3) | 1.87 (3) | 2.6642 (14) | 163 (2) |
C4—H4···O13viii | 0.93 | 2.43 | 3.164 (2) | 136 |
C10—H10A···O6ix | 0.93 | 2.45 | 3.344 (2) | 162 |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x, −y, −z; (iii) x, y−1, z; (iv) −x, −y, −z+1; (v) −x, −y+1, −z+1; (vi) x−1, y, z; (vii) −x, −y+1, −z; (viii) x, y, z+1; (ix) −x−1, −y, −z. |
Recently, we have reported the reactions between Co(NO3)2.6H2O and two proton-transfer compounds: (GH)2(pydc) (where G is guanidine) and (pipzH2)(pydc) (where pipz is piperazine) in a 1:2 molar ratio. These reactions lead to the formation of the complexes (GH)2[Co(H2O)6][Co(pydc)2]2 (Sheshmani et al., 2006) and (pipzH2)[Co(H2O)6][Co(pydc)2]2.8H2O (Aghabozorg, Attar Gharamaleki et al., 2007), respectively.
Here, we report the synthesis and X-ray crystal structure of the title compound (Fig. 1). The compound contains [Co(pydc)2]2- anions, [Co(H2O)6]2+ cations (site symmetry 1), and (tataH)+ cations. In the [Co(pydc)2]2- anions, the CoII atom is hexacoordinated by two N atoms (N1 and N2) and four O atoms (O1, O3, O5 and O7) from the carboxylate groups of two (pydc)2- groups that act as tridentate ligands. The coordination geometry is distorted octahedral, with atoms N1 and N2 occupying axial positions and the O atoms forming the equatorial plane. The N1—Co2—N2 angle deviates ca 7.7° from linearity. The mean Co—N and Co—O bond lengths for Co1 are 2.0214 (11) and 2.1658 (10) Å, respectively, consistent with similar complexes in the literature. The dihedral angle between the mean planes of the two (pydc)2- groups is 82.3 (1)°.
There is extensive O—H···O, N—H···O, N—H···N and C—H···O hydrogen bonding in the structure, as well as π–π stacking between (pydc)2- ligands with an interplanar distance of 3.484 (15) Å (symmetry operator: -x, -y + 1, -z + 1). Atom O8 of the C14?O8 carboxyl group lies above the N2/C9–C13 ring with an O···centroid distance of 3.240 (1) Å (symmetry operator: x, -y + 1, -z).