The polymeric title compound, {[Co(C4H4N2)(H2O)4](C8H4O4)}n, when refined in Imm2 from the diffraction intensities originally used for refinement in Immm [Yang, Li, Cao & Yao (2003). Acta Cryst. E59, m961–m963], is an ordered structure whose CoII atom, pyrazine ligand and phthalate counter-ion lie on special positions. The metal atom and N-heterocycle have mm2 site symmetry and the dianion m site symmetry.
Supporting information
CCDC reference: 289656
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.004 Å
- R factor = 0.023
- wR factor = 0.074
- Data-to-parameter ratio = 11.6
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat
O1W -H1W1 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat
O1W -H1# 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.87(3), Rep 1.870(10) ...... 3.00 su-Rat
H1# -O1 1.555 1.555
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio
Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
From the CIF: _diffrn_reflns_theta_max 27.50
From the CIF: _reflns_number_total 871
Count of symmetry unique reflns 483
Completeness (_total/calc) 180.33%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 388
Fraction of Friedel pairs measured 0.803
Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
7 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
4 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
0 ALERT type 3 Indicator that the structure quality may be low
4 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 the Zn analog; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
catena-poly[[tetraaquacobalt(II)-µ-pyrazine] phthalate]
top
Crystal data top
[Co(C4H4N2)(H2O)4](C8H4O4) | F(000) = 386 |
Mr = 375.20 | Dx = 1.794 Mg m−3 |
Orthorhombic, Imm2 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: I 2 -2 | Cell parameters from 2933 reflections |
a = 9.4033 (6) Å | θ = 2.9–28.4° |
b = 10.2886 (7) Å | µ = 1.28 mm−1 |
c = 7.1791 (5) Å | T = 298 K |
V = 694.55 (8) Å3 | Prism, orange |
Z = 2 | 0.45 × 0.28 × 0.27 mm |
Data collection top
Bruker APEX area-detector diffractometer | 871 independent reflections |
Radiation source: fine-focus sealed tube | 871 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.018 |
φ and ω scans | θmax = 27.5°, θmin = 2.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −12→11 |
Tmin = 0.545, Tmax = 0.723 | k = −13→13 |
2928 measured reflections | l = −9→9 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.023 | All H-atom parameters refined |
wR(F2) = 0.074 | w = 1/[σ2(Fo2) + (0.0542P)2 + 0.0753P] where P = (Fo2 + 2Fc2)/3 |
S = 1.25 | (Δ/σ)max = 0.001 |
871 reflections | Δρmax = 0.35 e Å−3 |
75 parameters | Δρmin = −0.51 e Å−3 |
3 restraints | Absolute structure: Flack (1983), 391 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.02 (1) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | 0.0000 | 0.5000 | 0.5000 | 0.0157 (2) | |
O1 | 0.3824 (2) | 0.3210 (2) | 0.7105 (2) | 0.0295 (4) | |
O1w | 0.1514 (1) | 0.3566 (1) | 0.4907 (3) | 0.0273 (3) | |
N1 | 0.0000 | 0.5000 | 0.1944 (5) | 0.0201 (8) | |
N2 | 0.0000 | 0.5000 | −0.1952 (5) | 0.0199 (9) | |
C1 | 0.1198 (3) | 0.5000 | 0.0970 (4) | 0.0239 (7) | |
C2 | 0.1207 (4) | 0.5000 | −0.0949 (4) | 0.0243 (8) | |
C3 | 0.5000 | 0.4334 (3) | 0.1354 (4) | 0.0263 (6) | |
C4 | 0.5000 | 0.3668 (4) | 0.3017 (5) | 0.0290 (8) | |
C5 | 0.5000 | 0.4321 (2) | 0.4697 (3) | 0.0175 (5) | |
C6 | 0.5000 | 0.3529 (3) | 0.6460 (4) | 0.0181 (6) | |
H1w1 | 0.220 (3) | 0.342 (3) | 0.563 (4) | 0.050 (9)* | |
H1w2 | 0.140 (4) | 0.301 (2) | 0.407 (3) | 0.039 (8)* | |
H1 | 0.2061 | 0.5000 | 0.1603 | 0.029* | |
H2 | 0.2075 | 0.5000 | −0.1569 | 0.029* | |
H3 | 0.5000 | 0.3881 | 0.0233 | 0.032* | |
H4 | 0.5000 | 0.2765 | 0.3009 | 0.035* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0168 (2) | 0.0183 (2) | 0.0119 (2) | 0.000 | 0.000 | 0.000 |
O1 | 0.0229 (7) | 0.0400 (9) | 0.0255 (8) | 0.0013 (6) | 0.0006 (6) | 0.0126 (7) |
O1w | 0.0272 (6) | 0.0275 (6) | 0.0271 (7) | 0.0085 (5) | −0.0064 (7) | −0.0072 (8) |
N1 | 0.021 (2) | 0.025 (2) | 0.015 (2) | 0.000 | 0.000 | 0.000 |
N2 | 0.022 (2) | 0.020 (2) | 0.017 (2) | 0.000 | 0.000 | 0.000 |
C1 | 0.018 (2) | 0.034 (2) | 0.020 (2) | 0.000 | 0.000 (1) | 0.000 |
C2 | 0.021 (2) | 0.037 (2) | 0.015 (2) | 0.000 | 0.003 (1) | 0.000 |
C3 | 0.033 (1) | 0.033 (2) | 0.013 (1) | 0.000 | 0.000 | −0.005 (1) |
C4 | 0.046 (2) | 0.020 (1) | 0.021 (2) | 0.000 | 0.000 | −0.001 (1) |
C5 | 0.019 (1) | 0.020 (1) | 0.014 (2) | 0.000 | 0.000 | 0.003 (1) |
C6 | 0.023 (1) | 0.015 (1) | 0.016 (1) | 0.000 | 0.000 | −0.001 (1) |
Geometric parameters (Å, º) top
Co1—O1w | 2.051 (1) | C3—C3vi | 1.370 (6) |
Co1—O1wi | 2.051 (1) | C3—C4 | 1.377 (5) |
Co1—O1wii | 2.051 (1) | C4—C5 | 1.380 (4) |
Co1—O1wiii | 2.051 (1) | C5—C5vi | 1.397 (5) |
Co1—N1 | 2.194 (4) | C5—C6 | 1.506 (4) |
Co1—N2iv | 2.188 (4) | C6—O1vii | 1.243 (2) |
O1—C6 | 1.243 (2) | O1w—H1w1 | 0.84 (1) |
N1—C1i | 1.326 (4) | O1w—H1w2 | 0.83 (1) |
N1—C1 | 1.326 (4) | C1—H1 | 0.93 |
N2—C2 | 1.344 (4) | C2—H2 | 0.93 |
N2—C2i | 1.344 (4) | C3—H3 | 0.93 |
N2—Co1v | 2.188 (4) | C4—H4 | 0.93 |
C1—C2 | 1.378 (3) | | |
| | | |
O1w—Co1—O1wi | 176.3 (1) | N1—C1—C2 | 122.2 (4) |
O1w—Co1—O1wii | 87.9 (1) | N2—C2—C1 | 122.1 (4) |
O1w—Co1—O1wiii | 92.0 (1) | C3vi—C3—C4 | 119.8 (2) |
O1w—Co1—N1 | 88.1 (1) | C3—C4—C5 | 121.1 (3) |
O1w—Co1—N2iv | 91.9 (1) | C4—C5—C5vi | 119.1 (2) |
O1wi—Co1—O1wii | 92.0 (1) | C4—C5—C6 | 118.1 (3) |
O1wi—Co1—O1wiii | 87.9 (1) | C5vi—C5—C6 | 122.8 (1) |
O1wi—Co1—N1 | 88.1 (1) | O1—C6—O1vii | 125.7 (3) |
O1wi—Co1—N2iv | 91.9 (1) | O1—C6—C5 | 117.1 (1) |
O1wii—Co1—O1wiii | 176.3 (1) | O1vii—C6—C5 | 117.1 (1) |
O1wii—Co1—N1 | 88.1 (1) | Co1—O1w—H1w1 | 130 (2) |
O1wii—Co1—N2iv | 91.9 (1) | Co1—O1w—H1w2 | 115 (2) |
O1wiii—Co1—N1 | 88.1 (1) | H1w1—O1w—H1w2 | 115 (3) |
O1wiii—Co1—N2iv | 91.9 (1) | N1—C1—H1 | 118.9 |
N1—Co1—N2iv | 180 | C2—C1—H1 | 118.9 |
C1i—N1—C1 | 116.3 (4) | N2—C2—H2 | 119.0 |
C1i—N1—Co1 | 121.8 (2) | C1—C2—H2 | 119.0 |
C1—N1—Co1 | 121.8 (2) | C3vi—C3—H3 | 120.1 |
C2—N2—C2i | 115.2 (4) | C4—C3—H3 | 120.1 |
C2—N2—Co1v | 122.4 (2) | C3—C4—H4 | 119.5 |
C2i—N2—Co1v | 122.4 (2) | C5—C4—H4 | 119.5 |
| | | |
O1wii—Co1—N1—C1i | 46.04 (4) | C2i—N2—C2—C1 | 0.0 |
O1wiii—Co1—N1—C1i | −133.96 (4) | Co1v—N2—C2—C1 | 180.0 |
O1w—Co1—N1—C1i | 133.96 (4) | N1—C1—C2—N2 | 0.0 |
O1wi—Co1—N1—C1i | −46.04 (4) | C3vi—C3—C4—C5 | 0.0 |
O1wii—Co1—N1—C1 | −133.96 (4) | C3—C4—C5—C5vi | 0.0 |
O1wiii—Co1—N1—C1 | 46.04 (4) | C3—C4—C5—C6 | 180.0 |
O1w—Co1—N1—C1 | −46.04 (4) | C4—C5—C6—O1 | −88.7 (2) |
O1wi—Co1—N1—C1 | 133.96 (4) | C5vi—C5—C6—O1 | 91.3 (2) |
C1i—N1—C1—C2 | 0.0 | C4—C5—C6—O1vii | 88.7 (2) |
Co1—N1—C1—C2 | 180.0 | C5vi—C5—C6—O1vii | −91.3 (2) |
Symmetry codes: (i) −x, −y+1, z; (ii) −x, y, z; (iii) x, −y+1, z; (iv) x, y, z+1; (v) x, y, z−1; (vi) −x+1, −y+1, z; (vii) −x+1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O1 | 0.84 (1) | 1.87 (1) | 2.709 (2) | 174 (4) |
O1w—H1w2···O1viii | 0.83 (1) | 1.91 (1) | 2.736 (2) | 178 (3) |
Symmetry code: (viii) −x+1/2, −y+1/2, z−1/2. |