Poly[bis­(μ₃-pyridine-2-carboxyl­ato)iron(II)]

The title compound, [Fe(C₆(CH₄N₄O₂)₂]_n, has been prepared by a hydro­thermal reaction of iron(II) chloride and pyridine-2-carboxylic acid. The asymmetric unit contains one Fe^II atom and two pyridine-2-carboxyl­ate anions. The Fe^II atoms are linked via bridging pyridine-2-carboxyl­ate, yielding a layered structure. The coordination geometry about the Fe atom is distorted octa­hedral.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.036
• wR factor = 0.122
• Data-to-parameter ratio = 11.0

checkCIF/PLATON results

No syntax errors found



Alert level B
SYMMS02_ALERT_1_B  The unit-cell lengths a and c should not be equal for a
            monoclinic cell
  Cell      10.2210   10.9120   10.2210
  Angles    90.0000  108.0000   90.0000
PLAT411_ALERT_2_B Short Inter H...H Contact  H4A    ..  H9A     ..       2.03 Ang.

Alert level C
PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) .        400 Ang.
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.17 Ratio

   0 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
   2 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 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
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1999); 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.

Poly[bis(µ₃-pyridine-2-carboxylato)iron(II)]

Crystal data

[Fe(C6H4NO2)2]	F(000) = 608
Mr = 300.05	Dx = 1.838 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 1899 reflections
a = 10.221 (4) Å	θ = 1.8–25.0°
b = 10.912 (4) Å	µ = 1.40 mm^−1
c = 10.221 (4) Å	T = 298 K
β = 108.000 (1)°	Block, red
V = 1084.2 (7) Å^3	0.30 × 0.30 × 0.30 mm
Z = 4

Data collection

Bruker SMART CCD diffractometer	1754 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.023
Graphite monochromator	θmax = 25.0°, θmin = 2.1°
φ and ω scans	h = −10→12
5317 measured reflections	k = −12→12
1899 independent reflections	l = −12→9

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.036	H-atom parameters constrained
wR(F^2) = 0.122	w = 1/[σ^2(Fo^2) + (0.0853P)^2 + 1.7322P] where P = (Fo^2 + 2Fc^2)/3
S = 1.00	(Δ/σ)max = 0.001
1899 reflections	Δρmax = 0.64 e Å^−3
173 parameters	Δρmin = −0.74 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.009 (2)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Fe	−0.01009 (4)	0.63420 (4)	0.40215 (4)	0.0233 (2)
C1	0.2578 (3)	0.4840 (3)	0.5410 (3)	0.0218 (6)
C2	0.3221 (3)	0.3841 (3)	0.6434 (3)	0.0212 (6)
C3	0.4609 (3)	0.3555 (3)	0.6776 (3)	0.0282 (7)
H3A	0.5163	0.3996	0.6373	0.034*
C4	0.5174 (3)	0.2661 (3)	0.7669 (3)	0.0248 (6)
H4A	0.6100	0.2457	0.7884	0.030*
C5	0.4334 (3)	0.2076 (3)	0.8237 (3)	0.0332 (7)
H5A	0.4689	0.1452	0.8866	0.040*
C6	0.2958 (3)	0.2367 (3)	0.7921 (3)	0.0298 (7)
H6A	0.2415	0.1946	0.8353	0.036*
C7	0.0286 (3)	0.6613 (3)	0.1144 (3)	0.0246 (6)
C8	0.1330 (3)	0.6281 (3)	0.0420 (3)	0.0230 (6)
C9	0.2373 (3)	0.6760 (3)	−0.1197 (3)	0.0313 (7)
H9A	0.2451	0.7247	−0.1916	0.038*
C10	0.3269 (4)	0.5794 (3)	−0.0744 (4)	0.0367 (8)
H10A	0.3946	0.5656	−0.1160	0.044*
C11	0.3201 (3)	0.5048 (3)	0.0271 (3)	0.0310 (7)
H11A	0.3797	0.4389	0.0559	0.037*
C12	0.2219 (4)	0.5311 (3)	0.0851 (4)	0.0362 (8)
H12A	0.2137	0.4820	0.1565	0.043*
N1	0.2386 (3)	0.3241 (2)	0.7006 (3)	0.0230 (5)
N2	0.1391 (3)	0.7009 (2)	−0.0616 (3)	0.0250 (6)
O1	0.1331 (2)	0.50902 (19)	0.5335 (2)	0.0260 (5)
O2	0.3255 (2)	0.5338 (2)	0.4750 (2)	0.0338 (6)
O3	0.0248 (2)	0.5941 (2)	0.2128 (2)	0.0318 (5)
O4	−0.0412 (2)	0.7560 (2)	0.0730 (2)	0.0313 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe	0.0210 (3)	0.0253 (3)	0.0252 (3)	−0.00095 (15)	0.0096 (2)	0.00319 (15)
C1	0.0184 (13)	0.0244 (14)	0.0227 (14)	−0.0045 (11)	0.0067 (11)	−0.0018 (11)
C2	0.0201 (14)	0.0231 (14)	0.0211 (14)	−0.0018 (11)	0.0073 (11)	−0.0014 (11)
C3	0.0215 (15)	0.0340 (18)	0.0305 (16)	0.0022 (12)	0.0100 (13)	0.0032 (13)
C4	0.0150 (13)	0.0325 (16)	0.0262 (15)	0.0076 (12)	0.0054 (11)	0.0069 (12)
C5	0.0327 (17)	0.0349 (17)	0.0303 (17)	0.0093 (14)	0.0073 (13)	0.0094 (14)
C6	0.0317 (16)	0.0320 (17)	0.0285 (16)	0.0014 (13)	0.0132 (13)	0.0075 (13)
C7	0.0218 (14)	0.0317 (16)	0.0209 (14)	−0.0050 (13)	0.0076 (11)	−0.0022 (12)
C8	0.0228 (15)	0.0262 (15)	0.0206 (14)	−0.0011 (11)	0.0075 (12)	−0.0026 (11)
C9	0.0315 (16)	0.0370 (18)	0.0309 (16)	0.0043 (14)	0.0180 (14)	0.0036 (14)
C10	0.0311 (17)	0.043 (2)	0.0392 (19)	0.0081 (15)	0.0162 (14)	−0.0071 (16)
C11	0.0296 (16)	0.0267 (16)	0.0390 (18)	0.0150 (13)	0.0142 (14)	0.0049 (13)
C12	0.0386 (18)	0.0336 (18)	0.0382 (18)	0.0076 (15)	0.0147 (15)	0.0093 (15)
N1	0.0217 (12)	0.0253 (13)	0.0234 (12)	0.0007 (10)	0.0089 (10)	0.0017 (10)
N2	0.0266 (13)	0.0271 (13)	0.0239 (12)	0.0034 (10)	0.0115 (10)	0.0013 (10)
O1	0.0178 (10)	0.0275 (11)	0.0334 (12)	0.0019 (8)	0.0093 (9)	0.0102 (9)
O2	0.0263 (11)	0.0393 (13)	0.0398 (13)	−0.0008 (10)	0.0162 (10)	0.0126 (10)
O3	0.0389 (12)	0.0366 (13)	0.0240 (11)	−0.0018 (10)	0.0157 (9)	0.0040 (9)
O4	0.0296 (12)	0.0357 (13)	0.0356 (12)	0.0075 (10)	0.0201 (10)	0.0071 (10)

Geometric parameters (Å, º)

Fe—O3	2.119 (2)	C6—H6A	0.9300
Fe—O1	2.144 (2)	C7—O4	1.253 (4)
Fe—O4^i	2.219 (2)	C7—O3	1.255 (4)
Fe—O1^ii	2.228 (2)	C7—C8	1.519 (4)
Fe—N1^ii	2.291 (3)	C8—N2	1.341 (4)
Fe—N2^i	2.313 (3)	C8—C12	1.376 (5)
C1—O2	1.232 (4)	C9—N2	1.342 (4)
C1—O1	1.283 (3)	C9—C10	1.379 (5)
C1—C2	1.514 (4)	C9—H9A	0.9300
C2—N1	1.343 (4)	C10—C11	1.338 (5)
C2—C3	1.388 (4)	C10—H10A	0.9300
C3—C4	1.339 (4)	C11—C12	1.345 (5)
C3—H3A	0.9300	C11—H11A	0.9300
C4—C5	1.338 (5)	C12—H12A	0.9300
C4—H4A	0.9300	N1—Fe^ii	2.291 (3)
C5—C6	1.379 (5)	N2—Fe^iii	2.313 (3)
C5—H5A	0.9300	O1—Fe^ii	2.228 (2)
C6—N1	1.337 (4)	O4—Fe^iii	2.219 (2)
O3—Fe—O1	99.52 (9)	N1—C6—H6A	119.3
O3—Fe—O4^i	159.27 (9)	C5—C6—H6A	119.3
O1—Fe—O4^i	94.99 (9)	O4—C7—O3	126.8 (3)
O3—Fe—O1^ii	113.20 (9)	O4—C7—C8	116.4 (3)
O1—Fe—O1^ii	72.94 (9)	O3—C7—C8	116.8 (3)
O4^i—Fe—O1^ii	85.15 (8)	N2—C8—C12	121.4 (3)
O3—Fe—N1^ii	93.32 (9)	N2—C8—C7	117.1 (3)
O1—Fe—N1^ii	144.64 (9)	C12—C8—C7	121.4 (3)
O4^i—Fe—N1^ii	83.11 (9)	N2—C9—C10	121.1 (3)
O1^ii—Fe—N1^ii	71.71 (9)	N2—C9—H9A	119.5
O3—Fe—N2^i	91.04 (9)	C10—C9—H9A	119.5
O1—Fe—N2^i	96.12 (9)	C11—C10—C9	122.5 (3)
O4^i—Fe—N2^i	72.66 (8)	C11—C10—H10A	118.8
O1^ii—Fe—N2^i	154.48 (9)	C9—C10—H10A	118.8
N1^ii—Fe—N2^i	116.57 (10)	C10—C11—C12	115.9 (3)
O2—C1—O1	126.1 (3)	C10—C11—H11A	122.0
O2—C1—C2	120.0 (3)	C12—C11—H11A	122.0
O1—C1—C2	113.9 (2)	C11—C12—C8	122.1 (3)
N1—C2—C3	121.2 (3)	C11—C12—H12A	118.9
N1—C2—C1	117.0 (3)	C8—C12—H12A	118.9
C3—C2—C1	121.8 (3)	C6—N1—C2	116.9 (3)
C4—C3—C2	121.8 (3)	C6—N1—Fe^ii	128.7 (2)
C4—C3—H3A	119.1	C2—N1—Fe^ii	113.47 (19)
C2—C3—H3A	119.1	C8—N2—C9	116.9 (3)
C5—C4—C3	116.4 (3)	C8—N2—Fe^iii	113.45 (19)
C5—C4—H4A	121.8	C9—N2—Fe^iii	129.3 (2)
C3—C4—H4A	121.8	C1—O1—Fe	130.27 (19)
C4—C5—C6	122.2 (3)	C1—O1—Fe^ii	118.30 (18)
C4—C5—H5A	118.9	Fe—O1—Fe^ii	107.06 (9)
C6—C5—H5A	118.9	C7—O3—Fe	131.8 (2)
N1—C6—C5	121.4 (3)	C7—O4—Fe^iii	120.44 (18)

Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) −x, −y+1, −z+1; (iii) x, −y+3/2, z−1/2.