4,4′-Bipyridinium(2+) hexa­aqua­iron(II) disulfate dihydrate

Fu, Y.-L.; Xu, Z.-W.; Ren, J.-L.; Ng, S.W.

doi:10.1107/S1600536805023391

4,4'-Bipyridinium(2+) hexaaquairon(II) disulfate dihydrate

Y.-L. Fu, Z.-W. Xu, J.-L. Ren and S. W. Ng

In the crystal structure of the title compound, (C₁₀H₁₀N₂)[Fe(H₂O)₆](SO₄)₂·2H₂O, hydrogen bonds link the 4,4'-bipyridinium cation, which lies on a special position of site symmetry 2, the hexaaquairon(II) cation, which lies on a center of symmetry, the sulfate anions and the uncoordinated water molecules into a three-dimensional network structure.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805023391/is6106sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536805023391/is6106Isup2.hkl Contains datablock I

CCDC reference: 282524

checkCIF report

Key indicators

Single-crystal X-ray study
T = 295 K
Mean (C-C) = 0.004 Å
R factor = 0.054
wR factor = 0.130
Data-to-parameter ratio = 12.8

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT731_ALERT_1_B Bond    Calc     0.86(5), Rep   0.850(10) ......       5.00 su-Rat
              N1   -H1N     1.555   1.555
PLAT735_ALERT_1_B D-H     Calc     0.86(5), Rep   0.850(10) ......       5.00 su-Rat
              N1   -H1N     1.555   1.555

Alert level C
ABSTM02_ALERT_3_C  The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
            Tmin and Tmax reported:      0.750     0.861
            Tmin(prime) and Tmax expected:      0.836     0.857
            RR(prime) =      0.892
            Please check that your absorption correction is appropriate.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large .............       0.89
PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct...          4
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Fe1
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          8
PLAT731_ALERT_1_C Bond    Calc     0.86(3), Rep   0.860(10) ......       3.00 su-Rat
              O1W  -H1W1    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.86(3), Rep   0.850(10) ......       3.00 su-Rat
              O1W  -H1W2    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(3), Rep   0.850(10) ......       3.00 su-Rat
              O2W  -H2W2    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O3W  -H3W1    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O3W  -H3W2    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.84(4), Rep   0.850(10) ......       4.00 su-Rat
              O4W  -H4W1    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(3), Rep   0.850(10) ......       3.00 su-Rat
              O4W  -H4W2    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.95(3), Rep   0.950(10) ......       3.00 su-Rat
              C1   -H1      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.95(3), Rep   0.950(10) ......       3.00 su-Rat
              C2   -H2      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.95(3), Rep   0.950(10) ......       3.00 su-Rat
              C4   -H4      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.95(3), Rep   0.950(10) ......       3.00 su-Rat
              C5   -H5      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.86(3), Rep   0.860(10) ......       3.00 su-Rat
              O1W  -H1#     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.86(3), Rep   0.850(10) ......       3.00 su-Rat
              O1W  -H2#     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(3), Rep   0.850(10) ......       3.00 su-Rat
              O2W  -H4#     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O3W  -H5#     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(4), Rep   0.850(10) ......       4.00 su-Rat
              O3W  -H6#     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.84(4), Rep   0.850(10) ......       4.00 su-Rat
              O4W  -H7#     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(3), Rep   0.850(10) ......       3.00 su-Rat
              O4W  -H8#     1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     1.88(3), Rep   1.880(10) ......       3.00 su-Rat
              H2#  -O4      1.555   8.557
PLAT736_ALERT_1_C H...A   Calc     1.93(3), Rep   1.930(10) ......       3.00 su-Rat
              H4#  -O3      1.555   2.564
PLAT736_ALERT_1_C H...A   Calc     1.92(4), Rep   1.920(10) ......       4.00 su-Rat
              H5#  -O2      1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     1.86(4), Rep   1.860(10) ......       4.00 su-Rat
              H6#  -O4W     1.555   5.666
PLAT736_ALERT_1_C H...A   Calc     1.89(3), Rep   1.890(10) ......       3.00 su-Rat
              H8#  -O4      1.555   6.657

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

  26 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
   2 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

4,4'-Bipyridinium(2+) hexaaquairon(II) disulfate dihydrate top

Crystal data top

(C₁₀H₁₀N₂)[Fe(H₂O)₆](SO₄)₂·2H₂O	F(000) = 1144
M_r = 550.30	D_x = 1.681 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 3298 reflections
a = 17.543 (1) Å	θ = 2.4–26.5°
b = 9.0676 (6) Å	µ = 0.97 mm⁻¹
c = 13.7592 (9) Å	T = 295 K
β = 96.670 (1)°	Block, colorless
V = 2173.9 (2) Å³	0.18 × 0.18 × 0.16 mm
Z = 4

Data collection top

Bruker APEX area-detector diffractometer	2482 independent reflections
Radiation source: fine-focus sealed tube	2310 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.042
φ and ω scans	θ_max = 27.5°, θ_min = 2.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −22→22
T_min = 0.750, T_max = 0.861	k = −11→11
11660 measured reflections	l = −17→17

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)] = 0.054	Hydrogen site location: difference Fourier map
wR(F²) = 0.130	All H-atom parameters refined
S = 1.21	w = 1/[σ²(F_o²) + (0.0639P)² + 2.4914P] where P = (F_o² + 2F_c²)/3
2482 reflections	(Δ/σ)_max = 0.001
194 parameters	Δρ_max = 0.35 e Å⁻³
17 restraints	Δρ_min = −0.88 e Å⁻³

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe1	0.2500	0.7500	0.5000	0.0252 (2)
S1	0.33598 (4)	0.29023 (8)	0.66964 (5)	0.0232 (2)
O1	0.3052 (1)	0.1908 (3)	0.5897 (2)	0.0360 (5)
O2	0.3904 (1)	0.3930 (2)	0.6314 (2)	0.0350 (5)
O3	0.2725 (1)	0.3738 (3)	0.7038 (2)	0.0418 (6)
O4	0.3744 (1)	0.2023 (3)	0.7500 (2)	0.0383 (5)
O1w	0.2111 (1)	0.6116 (2)	0.6070 (2)	0.0336 (5)
O2w	0.2182 (2)	0.6009 (3)	0.3853 (2)	0.0605 (8)
O3w	0.3608 (2)	0.6520 (3)	0.5282 (2)	0.0595 (8)
O4w	0.5302 (2)	0.2785 (4)	0.5877 (2)	0.0525 (7)
N1	0.3795 (2)	0.2184 (4)	0.4311 (2)	0.0397 (7)
C1	0.3814 (2)	0.3373 (4)	0.3754 (3)	0.0427 (8)
C2	0.4291 (2)	0.3422 (4)	0.3032 (2)	0.0372 (7)
C3	0.4743 (2)	0.2201 (3)	0.2891 (2)	0.0284 (6)
C4	0.4706 (2)	0.0980 (4)	0.3487 (2)	0.0340 (7)
C5	0.4233 (2)	0.1006 (4)	0.4209 (2)	0.0393 (8)
H1	0.347 (2)	0.410 (3)	0.394 (3)	0.05 (1)*
H2	0.429 (2)	0.424 (3)	0.260 (2)	0.05 (1)*
H4	0.501 (2)	0.014 (3)	0.340 (3)	0.04 (1)*
H5	0.422 (2)	0.018 (3)	0.463 (2)	0.05 (1)*
H1w1	0.237 (2)	0.536 (3)	0.630 (3)	0.07 (1)*
H1w2	0.184 (2)	0.642 (4)	0.651 (2)	0.05 (1)*
H2w1	0.209 (2)	0.511 (2)	0.394 (2)	0.05 (12)*
H2w2	0.235 (2)	0.612 (4)	0.330 (2)	0.07 (1)*
H3w1	0.371 (3)	0.577 (4)	0.564 (3)	0.11 (2)*
H3w2	0.398 (2)	0.667 (4)	0.495 (3)	0.06 (1)*
H4w1	0.490 (2)	0.325 (5)	0.597 (3)	0.07 (1)*
H4w2	0.559 (2)	0.268 (4)	0.641 (2)	0.06 (2)*
H1n	0.347 (3)	0.212 (6)	0.473 (3)	0.10 (2)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.0327 (3)	0.0224 (3)	0.0220 (3)	0.0016 (2)	0.0096 (2)	−0.0006 (2)
S1	0.0266 (4)	0.0250 (3)	0.0188 (3)	0.0009 (3)	0.0054 (2)	0.0021 (2)
O1	0.045 (1)	0.038 (1)	0.026 (1)	−0.010 (1)	0.010 (1)	−0.002 (1)
O2	0.034 (1)	0.032 (1)	0.040 (1)	−0.004 (1)	0.010 (1)	0.005 (1)
O3	0.046 (1)	0.046 (1)	0.037 (1)	0.014 (1)	0.021 (1)	0.006 (1)
O4	0.038 (1)	0.045 (1)	0.031 (1)	0.002 (1)	0.000 (1)	0.012 (1)
O1w	0.041 (1)	0.030 (1)	0.032 (1)	0.005 (1)	0.017 (1)	0.006 (1)
O2w	0.118 (3)	0.035 (1)	0.032 (1)	−0.027 (2)	0.027 (2)	−0.009 (1)
O3w	0.043 (2)	0.065 (2)	0.076 (2)	0.022 (1)	0.030 (1)	0.038 (2)
O4w	0.034 (1)	0.085 (2)	0.040 (2)	0.012 (1)	0.008 (1)	0.009 (1)
N1	0.035 (2)	0.061 (2)	0.026 (1)	−0.014 (1)	0.011 (1)	−0.009 (1)
C1	0.041 (2)	0.049 (2)	0.040 (2)	0.004 (2)	0.015 (2)	−0.006 (2)
C2	0.046 (2)	0.036 (2)	0.033 (2)	0.005 (1)	0.017 (1)	0.002 (1)
C3	0.030 (2)	0.032 (2)	0.024 (1)	−0.004 (1)	0.007 (1)	−0.001 (1)
C4	0.038 (2)	0.032 (2)	0.033 (2)	−0.003 (1)	0.007 (1)	0.003 (1)
C5	0.043 (2)	0.046 (2)	0.029 (2)	−0.016 (2)	0.006 (1)	0.005 (1)

Geometric parameters (Å, º) top

Fe1—O1w	2.107 (2)	C3—C3ⁱⁱ	1.481 (5)
Fe1—O1wⁱ	2.107 (2)	C4—C5	1.367 (4)
Fe1—O2w	2.103 (2)	O1w—H1w1	0.86 (1)
Fe1—O2wⁱ	2.103 (2)	O1w—H1w2	0.85 (1)
Fe1—O3w	2.132 (2)	O2w—H2w1	0.85 (1)
Fe1—O3wⁱ	2.132 (2)	O2w—H2w2	0.85 (1)
S1—O4	1.463 (2)	O3w—H3w1	0.85 (1)
S1—O3	1.469 (2)	O3w—H3w2	0.85 (1)
S1—O2	1.474 (2)	O4w—H4w1	0.85 (1)
S1—O1	1.475 (2)	O4w—H4w2	0.85 (1)
N1—C1	1.326 (5)	N1—H1n	0.85 (1)
N1—C5	1.333 (5)	C1—H1	0.95 (1)
C1—C2	1.371 (4)	C2—H2	0.95 (1)
C2—C3	1.389 (4)	C4—H4	0.95 (1)
C3—C4	1.384 (4)	C5—H5	0.95 (1)

O1w—Fe1—O1wⁱ	180	C4—C3—C3ⁱⁱ	120.3 (2)
O1w—Fe1—O2w	93.6 (1)	C2—C3—C3ⁱⁱ	120.5 (2)
O1w—Fe1—O2wⁱ	86.4 (1)	C5—C4—C3	119.4 (3)
O1w—Fe1—O3w	89.2 (1)	N1—C5—C4	119.8 (3)
O1w—Fe1—O3wⁱ	90.8 (1)	Fe1—O1w—H1w1	122 (2)
O1wⁱ—Fe1—O2w	86.4 (1)	Fe1—O1w—H1w2	123 (2)
O2wⁱ—Fe1—O1wⁱ	93.6 (1)	H1w1—O1w—H1w2	108 (2)
O1wⁱ—Fe1—O3w	90.8 (1)	Fe1—O2w—H2w1	124 (2)
O1wⁱ—Fe1—O3wⁱ	89.2 (1)	Fe1—O2w—H2w2	120 (3)
O2w—Fe1—O2wⁱ	180	H2w1—O2w—H2w2	110 (2)
O2w—Fe1—O3w	91.5 (1)	Fe1—O3w—H3w1	124 (3)
O2w—Fe1—O3wⁱ	88.6 (1)	Fe1—O3w—H3w2	125 (3)
O2wⁱ—Fe1—O3wⁱ	91.5 (1)	H3w1—O3w—H3w2	109 (2)
O2wⁱ—Fe1—O3w	88.6 (1)	H4w1—O4w—H4w2	110 (2)
O3w—Fe1—O3wⁱ	180	C1—N1—H1n	120 (4)
O4—S1—O3	109.9 (1)	C5—N1—H1n	117 (4)
O4—S1—O2	110.7 (1)	N1—C1—H1	111 (2)
O3—S1—O2	109.6 (1)	C2—C1—H1	129 (2)
O4—S1—O1	109.1 (1)	C1—C2—H2	121 (2)
O3—S1—O1	109.2 (1)	C3—C2—H2	120 (2)
O2—S1—O1	108.4 (1)	C5—C4—H4	121 (2)
C1—N1—C5	122.5 (3)	C3—C4—H4	120 (2)
N1—C1—C2	120.2 (3)	N1—C5—H5	121 (2)
C1—C2—C3	118.8 (3)	C4—C5—H5	120 (2)
C4—C3—C2	119.2 (3)

C5—N1—C1—C2	0.5 (5)	C2—C3—C4—C5	−0.7 (5)
N1—C1—C2—C3	0.9 (5)	C3ⁱⁱ—C3—C4—C5	179.5 (3)
C1—C2—C3—C4	−0.8 (5)	C1—N1—C5—C4	−2.1 (5)
C1—C2—C3—C3ⁱⁱ	179.0 (4)	C3—C4—C5—N1	2.1 (5)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H1w1···O3	0.86 (1)	1.86 (2)	2.692 (3)	164 (3)
O1w—H1w2···O4ⁱⁱⁱ	0.85 (1)	1.88 (1)	2.736 (3)	178 (3)
O2w—H2w1···O1^iv	0.85 (1)	1.86 (1)	2.705 (3)	176 (4)
O2w—H2w2···O3^v	0.85 (1)	1.93 (1)	2.783 (3)	177 (3)
O3w—H3w1···O2	0.85 (1)	1.92 (1)	2.762 (3)	173 (6)
O3w—H3w2···O4w^vi	0.85 (1)	1.86 (1)	2.703 (4)	172 (4)
O4w—H4w1···O2	0.85 (1)	1.96 (2)	2.792 (3)	168 (5)
O4w—H4w2···O4^vii	0.85 (1)	1.89 (1)	2.720 (3)	168 (4)
N1—H1n···O1	0.85 (1)	1.86 (2)	2.680 (3)	162 (6)

Symmetry codes: (iii) −x+1/2, y+1/2, −z+3/2; (iv) −x+1/2, −y+1/2, −z+1; (v) x, −y+1, z−1/2; (vi) −x+1, −y+1, −z+1; (vii) −x+1, y, −z+3/2.

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4,4'-Bipyridinium(2+) hexa­aqua­iron(II) disulfate dihydrate

Supporting information

Key indicators

checkCIF/PLATON results

4,4'-Bipyridinium(2+) hexaaquairon(II) disulfate dihydrate