The Co(II) atom in polymeric {[Co2(C10H2O8)(C4H4N2)(H2O)4]·2H2O}n exists in an octahedral coordination environment defined by the two O atoms of a chelating carboxyl group, the O atom of a monodentate carboxyl group of another benzenetetracarboxylato unit, two water molecules and the N atom of the pyrazine. The tetraanionic ligand and the N-heterocycle are located on inversion centers. The layer structure is linked by hydrogen bonds into a network structure.
Supporting information
CCDC reference: 225649
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.004 Å
- R factor = 0.035
- wR factor = 0.082
- Data-to-parameter ratio = 12.3
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.97
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.04 Ratio
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 12
O3 -CO1 -N1 -C6 -66.30 0.80 2.667 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 17
O3 -CO1 -N1 -C7 103.00 0.80 2.667 1.555 1.555 1.555
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat
O2W -H2W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.84(4), Rep 0.840(10) ...... 4.00 su-Rat
O2W -H2W2 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.850(10) ...... 3.00 su-Rat
O3W -H3W1 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1W1 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(4), Rep 0.840(10) ...... 4.00 su-Rat
O2W -H2W2 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat
O2W -H2W1 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.850(10) ...... 3.00 su-Rat
O3W -H3W1 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.98(4), Rep 1.980(10) ...... 4.00 su-Rat
H2W2 -O1W 1.555 2.676
PLAT736_ALERT_1_C H...A Calc 1.89(4), Rep 1.890(10) ...... 4.00 su-Rat
H2W1 -O3W 1.555 1.455
PLAT764_ALERT_4_C Overcomplete CIF Bond list Detected (Rep/Expd) . 1.11 Ratio
1 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
19 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
13 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
5 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: Atomic coordinates taken from isomorphous Ni compound (Yang et al., 2003); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Tetraaqua-1,2,4,5-benzenetetracarboxylato(pyrazine)dicobalt(II) dihydrate
top
Crystal data top
[Co2(C10H2O8)(C4H4N2)(H2O)4]2H2O | Z = 1 |
Mr = 556.16 | F(000) = 282 |
Triclinic, P1 | Dx = 1.970 Mg m−3 |
a = 7.2342 (4) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.0693 (5) Å | Cell parameters from 3407 reflections |
c = 9.3975 (6) Å | θ = 2.3–28.3° |
α = 96.114 (1)° | µ = 1.85 mm−1 |
β = 102.350 (1)° | T = 298 K |
γ = 116.053 (1)° | Prism, red |
V = 468.71 (5) Å3 | 0.48 × 0.27 × 0.16 mm |
Data collection top
Bruker SMART APEX area-detector diffractometer | 2084 independent reflections |
Radiation source: fine-focus sealed tube | 1780 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
φ and ω scan | θmax = 27.5°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→9 |
Tmin = 0.406, Tmax = 0.744 | k = −10→10 |
4046 measured reflections | l = −12→12 |
Refinement top
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.082 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.95 | w = 1/[σ2(Fo2) + (0.0368P)2] where P = (Fo2 + 2Fc2)/3 |
2084 reflections | (Δ/σ)max = 0.001 |
169 parameters | Δρmax = 0.58 e Å−3 |
6 restraints | Δρmin = −0.56 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | 0.59863 (6) | 0.81673 (5) | 0.67725 (4) | 0.0166 (1) | |
O1 | 0.6569 (3) | 0.5746 (3) | 0.6870 (2) | 0.0210 (4) | |
O2 | 0.8620 (3) | 0.8419 (3) | 0.8516 (2) | 0.0219 (4) | |
O3 | 0.5967 (3) | 0.2952 (3) | 1.1917 (2) | 0.0223 (4) | |
O4 | 0.9069 (3) | 0.3398 (3) | 1.3400 (2) | 0.0320 (5) | |
N1 | 0.8300 (4) | 0.9316 (3) | 0.5603 (3) | 0.0210 (5) | |
O1w | 0.3430 (3) | 0.7086 (3) | 0.4829 (2) | 0.0214 (4) | |
O2w | 0.5962 (4) | 1.0663 (3) | 0.7297 (3) | 0.0293 (5) | |
O3w | 1.3414 (4) | 1.1001 (4) | 0.8937 (3) | 0.0429 (6) | |
C1 | 0.8078 (4) | 0.6723 (4) | 0.8059 (3) | 0.0158 (5) | |
C2 | 0.9101 (4) | 0.5805 (4) | 0.9022 (3) | 0.0163 (5) | |
C3 | 0.8154 (4) | 0.5053 (4) | 1.0089 (3) | 0.0192 (6) | |
C4 | 0.9025 (4) | 0.4239 (4) | 1.1074 (3) | 0.0167 (5) | |
C5 | 0.7962 (4) | 0.3456 (4) | 1.2231 (3) | 0.0189 (6) | |
C6 | 0.9991 (5) | 1.1008 (4) | 0.6194 (3) | 0.0255 (6) | |
C7 | 0.8319 (5) | 0.8298 (4) | 0.4400 (3) | 0.0259 (7) | |
H1w1 | 0.232 (3) | 0.683 (4) | 0.512 (3) | 0.03 (1)* | |
H1w2 | 0.297 (6) | 0.596 (2) | 0.438 (4) | 0.05 (1)* | |
H2w1 | 0.510 (5) | 1.084 (6) | 0.770 (4) | 0.07 (2)* | |
H2w2 | 0.624 (6) | 1.144 (5) | 0.674 (4) | 0.07 (1)* | |
H3w1 | 1.218 (3) | 1.023 (5) | 0.897 (5) | 0.06 (1)* | |
H3w2 | 1.424 (5) | 1.160 (5) | 0.980 (2) | 0.05 (1)* | |
H3 | 0.6907 | 0.5092 | 1.0150 | 0.023* | |
H6 | 1.0034 | 1.1752 | 0.7041 | 0.031* | |
H7 | 0.7166 | 0.7096 | 0.3955 | 0.031* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0166 (2) | 0.0233 (2) | 0.0167 (2) | 0.0122 (2) | 0.0091 (2) | 0.0098 (2) |
O1 | 0.020 (1) | 0.024 (1) | 0.021 (1) | 0.013 (1) | 0.004 (1) | 0.005 (1) |
O2 | 0.025 (1) | 0.022 (1) | 0.020 (1) | 0.013 (1) | 0.004 (1) | 0.005 (1) |
O3 | 0.017 (1) | 0.038 (1) | 0.022 (1) | 0.016 (1) | 0.013 (1) | 0.017 (1) |
O4 | 0.025 (1) | 0.059 (2) | 0.023 (1) | 0.023 (1) | 0.014 (1) | 0.024 (1) |
N1 | 0.020 (1) | 0.028 (1) | 0.020 (1) | 0.013 (1) | 0.011 (1) | 0.012 (1) |
O1w | 0.021 (1) | 0.026 (1) | 0.019 (1) | 0.011 (1) | 0.007 (1) | 0.006 (1) |
O2w | 0.043 (1) | 0.029 (1) | 0.033 (1) | 0.024 (1) | 0.022 (1) | 0.016 (1) |
O3w | 0.035 (2) | 0.059 (2) | 0.027 (1) | 0.018 (1) | 0.011 (1) | −0.001 (1) |
C1 | 0.014 (1) | 0.023 (1) | 0.017 (1) | 0.010 (1) | 0.011 (1) | 0.010 (1) |
C2 | 0.018 (1) | 0.020 (1) | 0.015 (1) | 0.011 (1) | 0.006 (1) | 0.005 (1) |
C3 | 0.017 (1) | 0.026 (2) | 0.021 (2) | 0.014 (1) | 0.009 (1) | 0.008 (1) |
C4 | 0.016 (1) | 0.020 (1) | 0.017 (1) | 0.009 (1) | 0.009 (1) | 0.007 (1) |
C5 | 0.022 (1) | 0.023 (1) | 0.020 (2) | 0.014 (1) | 0.012 (1) | 0.010 (1) |
C6 | 0.024 (2) | 0.030 (2) | 0.024 (2) | 0.012 (1) | 0.011 (1) | 0.006 (1) |
C7 | 0.023 (2) | 0.026 (2) | 0.026 (2) | 0.007 (1) | 0.012 (1) | 0.008 (1) |
Geometric parameters (Å, º) top
Co1—O1 | 2.179 (2) | C3—C4 | 1.389 (4) |
Co1—O2 | 2.147 (2) | C4—C2ii | 1.393 (4) |
Co1—O3i | 2.047 (2) | C4—C5 | 1.500 (3) |
Co1—O1w | 2.077 (2) | C6—C7iii | 1.370 (4) |
Co1—O2w | 2.030 (2) | C7—C6iii | 1.370 (4) |
Co1—N1 | 2.123 (2) | O1w—H1w1 | 0.85 (1) |
O1—C1 | 1.264 (3) | O1w—H1w2 | 0.84 (1) |
O2—C1 | 1.242 (3) | O2w—H2w1 | 0.85 (1) |
O3—C5 | 1.270 (3) | O2w—H2w2 | 0.84 (1) |
O4—C5 | 1.233 (3) | O3w—H3w1 | 0.85 (1) |
N1—C6 | 1.323 (4) | O3w—H3w2 | 0.84 (1) |
N1—C7 | 1.332 (4) | C3—H3 | 0.93 |
C1—C2 | 1.500 (3) | C6—H6 | 0.93 |
C2—C3 | 1.379 (3) | C7—H7 | 0.93 |
C2—C4ii | 1.393 (4) | | |
| | | |
O1—Co1—O2 | 60.5 (1) | C3—C2—C1 | 116.9 (2) |
O1—Co1—O3i | 84.6 (1) | C4ii—C2—C1 | 123.3 (2) |
O1—Co1—O1w | 100.7 (1) | C2—C3—C4 | 121.3 (2) |
O1—Co1—O2w | 163.7 (1) | C3—C4—C2ii | 118.9 (2) |
O1—Co1—N1 | 91.4 (1) | C3—C4—C5 | 119.8 (2) |
O2—Co1—O3i | 88.1 (1) | C2ii—C4—C5 | 121.3 (2) |
O2—Co1—O1w | 160.9 (1) | O4—C5—O3 | 125.7 (2) |
O2—Co1—O2w | 104.1 (1) | O4—C5—C4 | 118.7 (2) |
O2—Co1—N1 | 85.3 (1) | O3—C5—C4 | 115.6 (2) |
O3i—Co1—O1w | 93.4 (1) | N1—C6—C7iii | 122.2 (3) |
O3i—Co1—O2w | 90.1 (1) | N1—C7—C6iii | 121.1 (3) |
O3i—Co1—N1 | 173.3 (1) | Co1—O1w—H1w1 | 106 (2) |
O1w—Co1—O2w | 95.0 (1) | Co1—O1w—H1w2 | 117 (3) |
O1w—Co1—N1 | 92.7 (1) | H1w1—O1w—H1w2 | 94 (3) |
O2w—Co1—N1 | 92.3 (1) | Co1—O2w—H2w1 | 126 (3) |
C1—O1—Co1 | 88.3 (2) | Co1—O2w—H2w2 | 121 (3) |
C1—O2—Co1 | 90.3 (2) | H2w1—O2w—H2w2 | 105 (4) |
C5—O3—Co1i | 126.2 (2) | H3w1—O3w—H3w2 | 111 (4) |
C6—N1—C7 | 116.7 (2) | C2—C3—H3 | 119.3 |
C6—N1—Co1 | 119.8 (2) | C4—C3—H3 | 119.3 |
C7—N1—Co1 | 122.7 (2) | N1—C6—H6 | 118.9 |
O2—C1—O1 | 120.7 (2) | C7iii—C6—H6 | 118.9 |
O2—C1—C2 | 118.7 (2) | N1—C7—H7 | 119.4 |
O1—C1—C2 | 120.4 (2) | C6iii—C7—H7 | 119.4 |
C3—C2—C4ii | 119.7 (2) | | |
| | | |
O2w—Co1—O1—C1 | −16.0 (3) | Co1—O2—C1—C2 | −168.5 (2) |
O3i—Co1—O1—C1 | −87.6 (1) | Co1—O1—C1—O2 | −5.6 (2) |
O1w—Co1—O1—C1 | 180.0 (1) | Co1—O1—C1—C2 | 168.4 (2) |
N1—Co1—O1—C1 | 87.0 (2) | O2—C1—C2—C3 | 86.6 (3) |
O2—Co1—O1—C1 | 3.2 (1) | O1—C1—C2—C3 | −87.5 (3) |
O2w—Co1—O2—C1 | 171.3 (2) | O2—C1—C2—C4ii | −90.5 (3) |
O3i—Co1—O2—C1 | 81.7 (2) | O1—C1—C2—C4ii | 95.4 (3) |
O1w—Co1—O2—C1 | −13.0 (3) | C4ii—C2—C3—C4 | −0.2 (5) |
N1—Co1—O2—C1 | −97.5 (2) | C1—C2—C3—C4 | −177.5 (3) |
O1—Co1—O2—C1 | −3.2 (1) | C2—C3—C4—C2ii | 0.2 (5) |
O2w—Co1—N1—C6 | 44.4 (2) | C2—C3—C4—C5 | 179.3 (2) |
O3i—Co1—N1—C6 | −66.3 (8) | Co1i—O3—C5—O4 | −1.9 (4) |
O1w—Co1—N1—C6 | 139.5 (2) | Co1i—O3—C5—C4 | −179.9 (2) |
O2—Co1—N1—C6 | −59.6 (2) | C3—C4—C5—O4 | −153.3 (3) |
O1—Co1—N1—C6 | −119.8 (2) | C2ii—C4—C5—O4 | 25.8 (4) |
O2w—Co1—N1—C7 | −146.3 (2) | C3—C4—C5—O3 | 24.9 (4) |
O3i—Co1—N1—C7 | 103.0 (8) | C2ii—C4—C5—O3 | −156.1 (3) |
O1w—Co1—N1—C7 | −51.2 (2) | C7—N1—C6—C7iii | 0.5 (5) |
O2—Co1—N1—C7 | 109.8 (2) | Co1—N1—C6—C7iii | 170.5 (2) |
O1—Co1—N1—C7 | 49.5 (2) | C6—N1—C7—C6iii | −0.5 (5) |
Co1—O2—C1—O1 | 5.6 (2) | Co1—N1—C7—C6iii | −170.1 (2) |
Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) −x+2, −y+1, −z+2; (iii) −x+2, −y+2, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w2···O1iv | 0.84 (1) | 1.90 (2) | 2.645 (3) | 147 (3) |
O1w—H1w1···O4i | 0.85 (1) | 1.87 (2) | 2.645 (3) | 152 (3) |
O2w—H2w2···O1wv | 0.84 (1) | 1.98 (1) | 2.816 (3) | 171 (4) |
O2w—H2w1···O3wvi | 0.85 (1) | 1.89 (1) | 2.723 (3) | 167 (4) |
O3w—H3w1···O2 | 0.85 (1) | 2.25 (2) | 3.069 (3) | 165 (4) |
O3w—H3w2···O3vii | 0.84 (1) | 1.99 (1) | 2.833 (3) | 175 (4) |
Symmetry codes: (i) −x+1, −y+1, −z+2; (iv) −x+1, −y+1, −z+1; (v) −x+1, −y+2, −z+1; (vi) x−1, y, z; (vii) x+1, y+1, z. |