The title compound, {[Fe(C
10H
8N
2)(H
2O)
4](C
8H
4O
4)}
n or [Fe(bpy)(H
2O)
4](bdc) (bpy is 4,4′-bipyridine and bdc is benzene-1,4-dicarboxylate), contains one-dimensional chains of Fe
II centres bridged by bpy ligands along the
b axis, with the equatorial coordination of four water molecules completing the octahedral coordination. Non-coordinated bdc anions balance the charge of the Fe
II centres and bridge adjacent one-dimensional chains through an extensive hydrogen-bonding network. The compound crystallizes in the centrosymmetric space group
, which defines twofold axes along both the Fe–bpy chains and the bdc anions.
Supporting information
CCDC reference: 262259
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.002 Å
- R factor = 0.023
- wR factor = 0.064
- Data-to-parameter ratio = 14.0
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.21 Ratio
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 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
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 1997); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: ORTEP-3 (Farrugia, 1997) and WebLab ViewerPro 3.7 (Accelrys, 2001); software used to prepare material for publication: XCIF.
catena-poly[[[tetraaquairon(II)]-µ-4,4'-bipyridine]
benzene-1,4-dicarboxylate]
top
Crystal data top
[Fe(C10H8N2)(H2O)4](C8H4O4) | F(000) = 464 |
Mr = 448.21 | Dx = 1.689 Mg m−3 |
Monoclinic, P2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yc | Cell parameters from 889 reflections |
a = 6.9541 (12) Å | θ = 3.2–27.9° |
b = 11.465 (2) Å | µ = 0.91 mm−1 |
c = 12.059 (2) Å | T = 150 K |
β = 113.547 (3)° | Block, orange |
V = 881.4 (3) Å3 | 0.50 × 0.37 × 0.22 mm |
Z = 2 | |
Data collection top
Bruker SMART 1000 CCD area-detector diffractometer | 2075 independent reflections |
Radiation source: fine-focus sealed tube | 2005 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.017 |
ω scans | θmax = 28.0°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→8 |
Tmin = 0.733, Tmax = 0.819 | k = −15→15 |
8043 measured reflections | l = −15→15 |
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)] = 0.023 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.065 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0212P)2 + 0.3552P] where P = (Fo2 + 2Fc2)/3 |
2075 reflections | (Δ/σ)max < 0.001 |
148 parameters | Δρmax = 0.26 e Å−3 |
6 restraints | Δρmin = −0.44 e Å−3 |
Special details top
Experimental. Crystal mounted in a thin film of perfluoropolyether oil on a mohair fibre. A
decay correction was carried out on the data. 172 reflections were remeasured
at the end of the collection with 0.00% calculated decay (within SAINT+
as part of the data reduction). |
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. Torsion angles of the bpy ligand were tabulated using RTAB: bpy:
20.48 (8) {C2 - C3 - C4 - C5} bpy-Fe-bpy: 20.58 (9) {C1 - N1 - N2_$1 - C6_$1} |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Fe1 | 0.5000 | 0.607200 (19) | 0.7500 | 0.01363 (9) | |
O1 | 0.78292 (15) | 0.62116 (8) | 0.90836 (8) | 0.01949 (19) | |
H1A | 0.871 (2) | 0.6560 (15) | 0.8951 (15) | 0.029* | |
H1B | 0.811 (3) | 0.6225 (14) | 0.9806 (12) | 0.029* | |
O2 | 0.30592 (15) | 0.59525 (8) | 0.84938 (9) | 0.01824 (19) | |
H2A | 0.243 (2) | 0.5359 (12) | 0.8438 (15) | 0.027* | |
H2B | 0.226 (2) | 0.6478 (13) | 0.8488 (15) | 0.027* | |
N1 | 0.5000 | 0.41972 (12) | 0.7500 | 0.0155 (3) | |
N2 | 0.5000 | −0.20021 (12) | 0.7500 | 0.0151 (3) | |
C1 | 0.59244 (19) | 0.35897 (11) | 0.85306 (10) | 0.0174 (2) | |
H1 | 0.6581 | 0.4008 | 0.9266 | 0.021* | |
C2 | 0.59655 (18) | 0.23832 (10) | 0.85715 (10) | 0.0165 (2) | |
H2 | 0.6643 | 0.1989 | 0.9321 | 0.020* | |
C3 | 0.5000 | 0.17500 (14) | 0.7500 | 0.0132 (3) | |
C4 | 0.5000 | 0.04574 (14) | 0.7500 | 0.0137 (3) | |
C5 | 0.53400 (18) | −0.01810 (10) | 0.85454 (10) | 0.0154 (2) | |
H5 | 0.5585 | 0.0212 | 0.9283 | 0.019* | |
C6 | 0.53211 (18) | −0.13899 (11) | 0.85098 (10) | 0.0165 (2) | |
H6 | 0.5546 | −0.1805 | 0.9233 | 0.020* | |
O11 | 0.10540 (15) | 1.38756 (7) | 0.84835 (8) | 0.0202 (2) | |
O12 | 0.05257 (14) | 0.77563 (8) | 0.85102 (8) | 0.01865 (19) | |
C11 | 0.0000 | 1.33655 (14) | 0.7500 | 0.0159 (3) | |
C12 | 0.0000 | 1.20380 (14) | 0.7500 | 0.0144 (3) | |
C13 | 0.04473 (18) | 1.14193 (11) | 0.85721 (10) | 0.0162 (2) | |
H13 | 0.0767 | 1.1830 | 0.9309 | 0.019* | |
C14 | 0.04279 (18) | 1.02034 (10) | 0.85686 (10) | 0.0155 (2) | |
H14 | 0.0709 | 0.9792 | 0.9301 | 0.019* | |
C15 | 0.0000 | 0.95856 (14) | 0.7500 | 0.0143 (3) | |
C16 | 0.0000 | 0.82673 (14) | 0.7500 | 0.0149 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.01718 (14) | 0.01038 (13) | 0.01280 (13) | 0.000 | 0.00543 (10) | 0.000 |
O1 | 0.0211 (5) | 0.0216 (5) | 0.0142 (4) | −0.0031 (3) | 0.0054 (4) | 0.0012 (3) |
O2 | 0.0229 (5) | 0.0132 (4) | 0.0214 (4) | −0.0001 (3) | 0.0118 (4) | −0.0003 (3) |
N1 | 0.0201 (7) | 0.0122 (6) | 0.0149 (7) | 0.000 | 0.0078 (6) | 0.000 |
N2 | 0.0164 (7) | 0.0123 (6) | 0.0159 (6) | 0.000 | 0.0056 (5) | 0.000 |
C1 | 0.0229 (6) | 0.0145 (5) | 0.0139 (5) | −0.0008 (5) | 0.0063 (5) | −0.0017 (4) |
C2 | 0.0196 (6) | 0.0144 (6) | 0.0141 (5) | 0.0007 (4) | 0.0054 (4) | 0.0010 (4) |
C3 | 0.0138 (7) | 0.0125 (7) | 0.0149 (7) | 0.000 | 0.0073 (6) | 0.000 |
C4 | 0.0125 (7) | 0.0125 (7) | 0.0160 (7) | 0.000 | 0.0057 (6) | 0.000 |
C5 | 0.0187 (6) | 0.0144 (5) | 0.0135 (5) | −0.0009 (4) | 0.0068 (4) | −0.0013 (4) |
C6 | 0.0189 (6) | 0.0148 (5) | 0.0158 (5) | 0.0002 (4) | 0.0067 (4) | 0.0018 (4) |
O11 | 0.0272 (5) | 0.0162 (4) | 0.0158 (4) | −0.0044 (3) | 0.0070 (4) | −0.0007 (3) |
O12 | 0.0235 (4) | 0.0156 (4) | 0.0164 (4) | 0.0008 (3) | 0.0075 (3) | 0.0021 (3) |
C11 | 0.0177 (8) | 0.0145 (8) | 0.0177 (7) | 0.000 | 0.0095 (6) | 0.000 |
C12 | 0.0136 (7) | 0.0134 (7) | 0.0157 (7) | 0.000 | 0.0054 (6) | 0.000 |
C13 | 0.0176 (5) | 0.0166 (5) | 0.0142 (5) | −0.0001 (4) | 0.0062 (4) | −0.0021 (4) |
C14 | 0.0165 (5) | 0.0166 (6) | 0.0131 (5) | 0.0012 (4) | 0.0058 (4) | 0.0020 (4) |
C15 | 0.0128 (7) | 0.0148 (8) | 0.0153 (7) | 0.000 | 0.0055 (6) | 0.000 |
C16 | 0.0135 (7) | 0.0149 (8) | 0.0164 (7) | 0.000 | 0.0061 (6) | 0.000 |
Geometric parameters (Å, º) top
Fe1—O1 | 2.1311 (10) | C3—C4 | 1.482 (2) |
Fe1—O1i | 2.1311 (10) | C4—C5 | 1.3939 (14) |
Fe1—O2i | 2.1374 (10) | C4—C5i | 1.3940 (14) |
Fe1—O2 | 2.1375 (10) | C5—C6 | 1.3866 (16) |
Fe1—N1 | 2.1495 (15) | C5—H5 | 0.9500 |
Fe1—N2ii | 2.2081 (14) | C6—H6 | 0.9500 |
O1—H1A | 0.797 (13) | O11—C11 | 1.2615 (12) |
O1—H1B | 0.813 (13) | O12—C16 | 1.2670 (11) |
O2—H2A | 0.796 (13) | C11—O11iv | 1.2614 (12) |
O2—H2B | 0.816 (13) | C11—C12 | 1.522 (2) |
N1—C1i | 1.3434 (14) | C12—C13 | 1.3965 (14) |
N1—C1 | 1.3434 (14) | C12—C13iv | 1.3965 (14) |
N2—C6i | 1.3447 (14) | C13—C14 | 1.3941 (16) |
N2—C6 | 1.3447 (14) | C13—H13 | 0.9500 |
N2—Fe1iii | 2.2081 (14) | C14—C15 | 1.3944 (14) |
C1—C2 | 1.3840 (17) | C14—H14 | 0.9500 |
C1—H1 | 0.9500 | C15—C14iv | 1.3944 (14) |
C2—C3 | 1.3980 (14) | C15—C16 | 1.511 (2) |
C2—H2 | 0.9500 | C16—O12iv | 1.2670 (11) |
C3—C2i | 1.3980 (14) | | |
| | | |
O1—Fe1—O1i | 171.39 (5) | C3—C2—H2 | 120.3 |
O1—Fe1—O2i | 86.77 (4) | C2i—C3—C2 | 117.42 (15) |
O1i—Fe1—O2i | 93.79 (4) | C2i—C3—C4 | 121.29 (7) |
O1—Fe1—O2 | 93.79 (4) | C2—C3—C4 | 121.29 (7) |
O1i—Fe1—O2 | 86.77 (4) | C5—C4—C5i | 116.64 (15) |
O2i—Fe1—O2 | 172.65 (5) | C5—C4—C3 | 121.68 (7) |
O1—Fe1—N1 | 94.31 (3) | C5i—C4—C3 | 121.68 (7) |
O1i—Fe1—N1 | 94.31 (3) | C6—C5—C4 | 120.06 (11) |
O2i—Fe1—N1 | 86.33 (2) | C6—C5—H5 | 120.0 |
O2—Fe1—N1 | 86.32 (2) | C4—C5—H5 | 120.0 |
O1—Fe1—N2ii | 85.69 (3) | N2—C6—C5 | 123.08 (11) |
O1i—Fe1—N2ii | 85.69 (3) | N2—C6—H6 | 118.5 |
O2i—Fe1—N2ii | 93.67 (2) | C5—C6—H6 | 118.5 |
O2—Fe1—N2ii | 93.68 (2) | O11iv—C11—O11 | 124.76 (15) |
N1—Fe1—N2ii | 180.0 | O11iv—C11—C12 | 117.62 (8) |
Fe1—O1—H1A | 111.4 (12) | O11—C11—C12 | 117.62 (8) |
Fe1—O1—H1B | 134.6 (13) | C13—C12—C13iv | 118.94 (15) |
H1A—O1—H1B | 109.2 (17) | C13—C12—C11 | 120.53 (8) |
Fe1—O2—H2A | 117.0 (12) | C13iv—C12—C11 | 120.53 (8) |
Fe1—O2—H2B | 121.7 (12) | C14—C13—C12 | 120.45 (11) |
H2A—O2—H2B | 106.6 (17) | C14—C13—H13 | 119.8 |
C1i—N1—C1 | 117.54 (15) | C12—C13—H13 | 119.8 |
C1i—N1—Fe1 | 121.23 (7) | C13—C14—C15 | 120.59 (11) |
C1—N1—Fe1 | 121.23 (7) | C13—C14—H14 | 119.7 |
C6i—N2—C6 | 117.07 (14) | C15—C14—H14 | 119.7 |
C6i—N2—Fe1iii | 121.46 (7) | C14iv—C15—C14 | 118.95 (15) |
C6—N2—Fe1iii | 121.46 (7) | C14iv—C15—C16 | 120.53 (8) |
N1—C1—C2 | 123.13 (11) | C14—C15—C16 | 120.53 (8) |
N1—C1—H1 | 118.4 | O12—C16—O12iv | 124.91 (15) |
C2—C1—H1 | 118.4 | O12—C16—C15 | 117.55 (8) |
C1—C2—C3 | 119.38 (11) | O12iv—C16—C15 | 117.55 (8) |
C1—C2—H2 | 120.3 | | |
Symmetry codes: (i) −x+1, y, −z+3/2; (ii) x, y+1, z; (iii) x, y−1, z; (iv) −x, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O12v | 0.80 (1) | 2.07 (1) | 2.8578 (13) | 168 (2) |
O1—H1B···O11vi | 0.81 (1) | 1.91 (1) | 2.7204 (14) | 174 (2) |
O2—H2A···O11iii | 0.80 (1) | 1.97 (1) | 2.7570 (13) | 174 (2) |
O2—H2B···O12 | 0.82 (1) | 1.91 (1) | 2.7220 (13) | 177 (2) |
Symmetry codes: (iii) x, y−1, z; (v) x+1, y, z; (vi) −x+1, −y+2, −z+2. |