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The title compound, [Fe(C10H6N4O4)2(H2O)]n, has been prepared from an aqueous solution of iron(II) chloride and pyrazine-2-carboxylic acid. The asymmetric unit contains one FeII, two pyrazine-2-carboxylate anions and one aqua ligand. The FeII atoms are linked via bridging pyrazine-2-carboxylate ligands, leading to a polymeric structure with zigzag-chains extending parallel to the b axis. The coordination of the Fe atom is distorted octahedral.
Supporting information
CCDC reference: 1218930
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.004 Å
- R factor = 0.028
- wR factor = 0.067
- Data-to-parameter ratio = 12.6
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT094_ALERT_2_B Ratio of Maximum / Minimum Residual Density .... 4.09
Alert level C
STRVA01_ALERT_4_C Flack test results are ambiguous.
From the CIF: _refine_ls_abs_structure_Flack 0.453
From the CIF: _refine_ls_abs_structure_Flack_su 0.018
PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.45
PLAT731_ALERT_1_C Bond Calc 0.90(4), Rep 0.899(18) ...... 2.22 su-Ra
O5 -H2W 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.90(4), Rep 0.899(18) ...... 2.22 su-Ra
O5 -H2W 1.555 1.555
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 26.50
From the CIF: _reflns_number_total 2370
Count of symmetry unique reflns 1392
Completeness (_total/calc) 170.26%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 978
Fraction of Friedel pairs measured 0.703
Are heavy atom types Z>Si present yes
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
2 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
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
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1999); software used to prepare material for publication: SHELXTL.
catena-Poly[[aqua(pyrazine-2-carboxylato)iron(II)]-µ-pyrazine-2-carboxylato]
top
Crystal data top
[Fe(C5H3N2O2)2(H2O)] | F(000) = 648 |
Mr = 320.05 | Dx = 1.853 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 3711 reflections |
a = 7.7905 (15) Å | θ = 3.0–28.0° |
b = 9.8787 (19) Å | µ = 1.34 mm−1 |
c = 14.909 (3) Å | T = 298 K |
V = 1147.4 (4) Å3 | Block, colorless |
Z = 4 | 0.10 × 0.10 × 0.10 mm |
Data collection top
Bruker SMART CCD diffractometer | 2370 independent reflections |
Radiation source: fine-focus sealed tube | 2215 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.026 |
φ and ω scans | θmax = 26.5°, θmin = 2.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1998) | h = −8→9 |
Tmin = 0.878, Tmax = 0.878 | k = −12→11 |
6291 measured reflections | l = −18→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)] = 0.028 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.067 | w = 1/[σ2(Fo2) + (0.0397P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.11 | (Δ/σ)max = 0.001 |
2370 reflections | Δρmax = 0.92 e Å−3 |
188 parameters | Δρmin = −0.22 e Å−3 |
3 restraints | Absolute structure: Flack (1983), 987 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.453 (18) |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Fe1 | 0.92677 (4) | 0.86587 (3) | 0.90929 (2) | 0.01634 (10) | |
C1 | 0.6949 (3) | 0.6917 (3) | 0.81677 (18) | 0.0256 (6) | |
C2 | 0.8718 (3) | 0.6453 (3) | 0.78893 (17) | 0.0247 (5) | |
C3 | 1.1637 (4) | 0.6690 (3) | 0.7994 (2) | 0.0305 (7) | |
H3 | 1.2596 | 0.7105 | 0.8244 | 0.037* | |
C4 | 0.6758 (4) | 1.0572 (3) | 1.0107 (2) | 0.0338 (7) | |
H4 | 0.5855 | 1.0223 | 0.9771 | 0.041* | |
C5 | 0.6419 (4) | 1.1486 (3) | 1.0787 (2) | 0.0396 (7) | |
H5A | 0.5287 | 1.1729 | 1.0901 | 0.047* | |
C6 | 0.9250 (4) | 1.1655 (3) | 1.1088 (2) | 0.0414 (8) | |
H6 | 1.0149 | 1.2024 | 1.1417 | 0.050* | |
C7 | 0.9625 (4) | 1.0736 (3) | 1.04108 (19) | 0.0307 (7) | |
C8 | 1.1428 (4) | 1.0284 (3) | 1.0192 (2) | 0.0311 (7) | |
C9 | 1.1056 (3) | 1.0420 (3) | 0.77249 (18) | 0.0274 (6) | |
H9 | 1.2015 | 0.9969 | 0.7946 | 0.033* | |
C10 | 0.8149 (4) | 1.0676 (3) | 0.7634 (2) | 0.0309 (6) | |
H10 | 0.7045 | 1.0422 | 0.7800 | 0.037* | |
N1 | 1.0062 (3) | 0.7082 (2) | 0.82476 (15) | 0.0271 (5) | |
N2 | 0.8353 (3) | 1.0188 (2) | 0.99261 (15) | 0.0278 (5) | |
N3 | 0.7655 (4) | 1.2026 (3) | 1.1282 (2) | 0.0480 (8) | |
N4 | 0.9498 (3) | 1.0048 (2) | 0.80113 (15) | 0.0283 (5) | |
O1 | 0.6940 (2) | 0.7973 (2) | 0.86886 (13) | 0.0294 (4) | |
O2 | 0.5688 (2) | 0.6303 (2) | 0.79086 (13) | 0.0389 (5) | |
O3 | 1.1535 (3) | 0.9350 (2) | 0.95922 (13) | 0.0297 (4) | |
O4 | 1.2623 (3) | 1.0798 (3) | 1.05891 (17) | 0.0524 (7) | |
O5 | 0.9186 (3) | 0.7349 (2) | 1.01670 (13) | 0.0364 (5) | |
H1W | 1.004 (3) | 0.721 (4) | 1.055 (2) | 0.080* | |
H2W | 0.838 (4) | 0.677 (4) | 1.036 (3) | 0.080* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.01506 (15) | 0.01734 (16) | 0.01661 (16) | 0.00004 (14) | 0.00058 (14) | −0.00064 (14) |
C1 | 0.0220 (13) | 0.0289 (14) | 0.0260 (14) | 0.0005 (11) | 0.0003 (11) | 0.0025 (11) |
C2 | 0.0262 (13) | 0.0263 (14) | 0.0215 (12) | −0.0035 (11) | −0.0013 (10) | 0.0019 (11) |
C3 | 0.0224 (14) | 0.0361 (18) | 0.0331 (15) | 0.0016 (12) | −0.0008 (12) | −0.0013 (12) |
C4 | 0.0270 (15) | 0.0336 (17) | 0.0408 (17) | −0.0026 (13) | −0.0014 (13) | −0.0007 (13) |
C5 | 0.0314 (15) | 0.0413 (18) | 0.0460 (18) | 0.0038 (14) | 0.0028 (14) | −0.0092 (16) |
C6 | 0.0336 (16) | 0.0449 (19) | 0.0457 (19) | −0.0025 (16) | −0.0062 (15) | −0.0149 (13) |
C7 | 0.0302 (17) | 0.0328 (15) | 0.0292 (15) | −0.0018 (12) | −0.0002 (11) | 0.0022 (12) |
C8 | 0.0280 (15) | 0.0331 (17) | 0.0322 (15) | 0.0009 (13) | −0.0031 (12) | 0.0024 (13) |
C9 | 0.0251 (15) | 0.0289 (14) | 0.0282 (14) | 0.0000 (11) | 0.0000 (11) | 0.0024 (11) |
C10 | 0.0228 (14) | 0.0353 (16) | 0.0347 (16) | −0.0015 (13) | −0.0009 (12) | 0.0045 (13) |
N1 | 0.0239 (11) | 0.0289 (13) | 0.0283 (13) | 0.0015 (10) | 0.0013 (10) | 0.0031 (10) |
N2 | 0.0259 (12) | 0.0279 (13) | 0.0294 (12) | −0.0002 (10) | −0.0008 (10) | −0.0006 (10) |
N3 | 0.0397 (16) | 0.0515 (19) | 0.0527 (17) | 0.0044 (14) | 0.0055 (13) | −0.0200 (14) |
N4 | 0.0287 (13) | 0.0287 (12) | 0.0277 (11) | −0.0001 (11) | −0.0007 (10) | 0.0017 (10) |
O1 | 0.0251 (10) | 0.0341 (11) | 0.0290 (10) | 0.0019 (9) | 0.0030 (8) | −0.0028 (9) |
O2 | 0.0252 (10) | 0.0460 (12) | 0.0454 (12) | −0.0052 (12) | 0.0007 (9) | −0.0107 (10) |
O3 | 0.0261 (10) | 0.0305 (11) | 0.0325 (11) | 0.0031 (9) | −0.0014 (8) | −0.0011 (9) |
O4 | 0.0301 (12) | 0.0648 (16) | 0.0624 (16) | −0.0043 (11) | −0.0079 (11) | −0.0226 (13) |
O5 | 0.0339 (11) | 0.0410 (12) | 0.0345 (11) | −0.0101 (11) | −0.0076 (10) | 0.0128 (9) |
Geometric parameters (Å, º) top
Fe1—O1 | 2.028 (2) | C5—N3 | 1.325 (4) |
Fe1—O3 | 2.035 (2) | C5—H5A | 0.9300 |
Fe1—O5 | 2.0594 (19) | C6—N3 | 1.328 (4) |
Fe1—N2 | 2.081 (2) | C6—C7 | 1.389 (4) |
Fe1—N1 | 2.097 (2) | C6—H6 | 0.9300 |
Fe1—N4 | 2.125 (2) | C7—N2 | 1.340 (4) |
C1—O2 | 1.218 (3) | C7—C8 | 1.510 (4) |
C1—O1 | 1.300 (3) | C8—O4 | 1.214 (4) |
C1—C2 | 1.510 (4) | C8—O3 | 1.288 (4) |
C2—N1 | 1.329 (3) | C9—N4 | 1.338 (3) |
C2—C9i | 1.383 (4) | C9—C2ii | 1.383 (4) |
C3—N1 | 1.340 (4) | C9—H9 | 0.9300 |
C3—C10i | 1.382 (4) | C10—N4 | 1.343 (4) |
C3—H3 | 0.9300 | C10—C3ii | 1.382 (4) |
C4—N2 | 1.327 (4) | C10—H10 | 0.9300 |
C4—C5 | 1.383 (4) | O5—H1W | 0.887 (18) |
C4—H4 | 0.9300 | O5—H2W | 0.899 (18) |
| | | |
O1—Fe1—O3 | 175.80 (8) | N3—C6—C7 | 122.4 (3) |
O1—Fe1—O5 | 89.64 (9) | N3—C6—H6 | 118.8 |
O3—Fe1—O5 | 87.31 (8) | C7—C6—H6 | 118.8 |
O1—Fe1—N2 | 96.54 (9) | N2—C7—C6 | 120.0 (3) |
O3—Fe1—N2 | 80.52 (9) | N2—C7—C8 | 116.9 (2) |
O5—Fe1—N2 | 88.92 (9) | C6—C7—C8 | 123.1 (3) |
O1—Fe1—N1 | 80.63 (8) | O4—C8—O3 | 126.1 (3) |
O3—Fe1—N1 | 102.28 (9) | O4—C8—C7 | 119.0 (3) |
O5—Fe1—N1 | 90.58 (9) | O3—C8—C7 | 115.0 (2) |
N2—Fe1—N1 | 177.13 (10) | N4—C9—C2ii | 122.0 (2) |
O1—Fe1—N4 | 93.77 (8) | N4—C9—H9 | 119.0 |
O3—Fe1—N4 | 89.29 (9) | C2ii—C9—H9 | 119.0 |
O5—Fe1—N4 | 176.59 (10) | N4—C10—C3ii | 121.6 (3) |
N2—Fe1—N4 | 90.75 (9) | N4—C10—H10 | 119.2 |
N1—Fe1—N4 | 89.92 (9) | C3ii—C10—H10 | 119.2 |
O2—C1—O1 | 125.8 (2) | C2—N1—C3 | 118.2 (2) |
O2—C1—C2 | 119.9 (2) | C2—N1—Fe1 | 110.85 (18) |
O1—C1—C2 | 114.4 (2) | C3—N1—Fe1 | 130.8 (2) |
N1—C2—C9i | 120.7 (2) | C4—N2—C7 | 117.9 (2) |
N1—C2—C1 | 117.8 (2) | C4—N2—Fe1 | 130.5 (2) |
C9i—C2—C1 | 121.5 (2) | C7—N2—Fe1 | 111.21 (19) |
N1—C3—C10i | 120.7 (3) | C5—N3—C6 | 116.6 (3) |
N1—C3—H3 | 119.6 | C9—N4—C10 | 116.7 (2) |
C10i—C3—H3 | 119.6 | C9—N4—Fe1 | 119.73 (18) |
N2—C4—C5 | 120.9 (3) | C10—N4—Fe1 | 123.36 (19) |
N2—C4—H4 | 119.5 | C1—O1—Fe1 | 116.13 (17) |
C5—C4—H4 | 119.5 | C8—O3—Fe1 | 116.00 (18) |
N3—C5—C4 | 122.2 (3) | Fe1—O5—H1W | 125 (2) |
N3—C5—H5A | 118.9 | Fe1—O5—H2W | 133 (2) |
C4—C5—H5A | 118.9 | H1W—O5—H2W | 103 (2) |
Symmetry codes: (i) −x+2, y−1/2, −z+3/2; (ii) −x+2, y+1/2, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H1W···O1iii | 0.89 (2) | 1.87 (2) | 2.759 (3) | 176 (4) |
O5—H2W···O3iv | 0.90 (2) | 1.81 (2) | 2.686 (3) | 163 (4) |
Symmetry codes: (iii) x+1/2, −y+3/2, −z+2; (iv) x−1/2, −y+3/2, −z+2. |
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