catena-Poly[hexa­methyl­enediaminium [ferrate(III)-μ-hydroxo-κ²O:O-di-μ-sulfato-κ⁴O:O′] monohydrate]

Ferric sulfate reacts with 1,6-diamino­hexa­ne in the presence of acid under hydro­thermal conditions to form the title compound, (C₆H₁₈N₂)[Fe(OH)(SO₄)₂]·H₂O. The six-coordinate ferrate trianion exists as a μ₂-hydroxodi-μ₂-sulfate-bridged chain that propagates along the b axis of the monoclinic unit cell. The dication and uncoordinated water mol­ecule connect the polyanionic chain into a three-dimensional network structure. The asymmetric unit contains two Fe ions, each on a center of symmetry.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.035
• wR factor = 0.100
• Data-to-parameter ratio = 16.8

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.97
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          8

Alert level G
FORMU01_ALERT_1_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety. This is
            usually due to the moiety formula being in the wrong format.
            Atom count from _chemical_formula_sum:   C6 H21 Fe1 N2 O10 S2
            Atom count from _chemical_formula_moiety:C6 H20 Fe1 N2 O10 S2

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   3 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
   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

---

Computing details

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.

catena-Poly[hexamethylenediaminium [ferrate(III)-µ-hydroxo-κ²O:O-di-µ-sulfato-κ⁴O:O'] monohydrate]

Crystal data

(C6H18N2)[Fe(OH)(SO4)2]·H2O	F(000) = 836
Mr = 401.22	Dx = 1.731 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 2196 reflections
a = 8.7918 (7) Å	θ = 2.5–28.3°
b = 6.9963 (5) Å	µ = 1.30 mm^−1
c = 25.032 (1) Å	T = 295 K
β = 90.289 (2)°	Block, colorless
V = 1539.68 (18) Å^3	0.35 × 0.12 × 0.12 mm
Z = 4

Data collection

Bruker APEX area-detector diffractometer	3439 independent reflections
Radiation source: fine-focus sealed tube	2483 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.027
φ and ω scans	θmax = 27.5°, θmin = 1.6°
Absorption correction: multi-scan (SADABS; Bruker, 2002)	h = −4→11
Tmin = 0.640, Tmax = 0.860	k = −8→9
8058 measured reflections	l = −31→32

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.035	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.100	H atoms treated by a mixture of independent and constrained refinement
S = 0.99	w = 1/[σ^2(Fo^2) + (0.0548P)^2] where P = (Fo^2 + 2Fc^2)/3
3439 reflections	(Δ/σ)max = 0.001
205 parameters	Δρmax = 0.34 e Å^−3
3 restraints	Δρmin = −0.43 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.5000	0.5000	0.5000	0.01567 (13)
Fe2	0.5000	1.0000	0.5000	0.01611 (14)
S1	0.31767 (7)	0.74565 (8)	0.58885 (2)	0.0196 (2)
S2	0.26738 (7)	0.76189 (8)	0.42675 (3)	0.0203 (2)
O1	0.4009 (2)	0.5741 (2)	0.5691 (1)	0.0300 (4)
O2	0.3330 (2)	0.9034 (2)	0.5488 (1)	0.0218 (4)
O3	0.1584 (2)	0.6972 (3)	0.5943 (1)	0.0389 (5)
O4	0.3861 (2)	0.8025 (3)	0.6388 (1)	0.0367 (5)
O5	0.3757 (2)	0.9234 (2)	0.4348 (1)	0.0218 (4)
O6	0.3203 (2)	0.5956 (2)	0.4584 (1)	0.0260 (4)
O7	0.2613 (3)	0.7110 (3)	0.3707 (1)	0.0413 (6)
O8	0.1185 (2)	0.8191 (3)	0.4464 (1)	0.0367 (5)
O9	0.6005 (2)	0.7503 (2)	0.4977 (1)	0.0183 (4)
O1w	0.8812 (2)	0.7911 (3)	0.5430 (1)	0.0433 (6)
N1	0.6995 (3)	0.6999 (3)	0.6367 (1)	0.0378 (6)
N2	1.3338 (3)	0.7646 (3)	0.9049 (1)	0.0309 (6)
C1	0.7605 (4)	0.7846 (4)	0.6864 (1)	0.0382 (7)
C2	0.9144 (3)	0.7019 (4)	0.7010 (1)	0.0372 (7)
C3	0.9737 (4)	0.7884 (4)	0.7524 (1)	0.0416 (8)
C4	1.1260 (4)	0.7073 (4)	0.7713 (1)	0.0377 (7)
C5	1.1650 (4)	0.7815 (4)	0.8266 (1)	0.0375 (7)
C6	1.3173 (3)	0.7146 (4)	0.8473 (1)	0.0299 (6)
H9o	0.685 (2)	0.752 (3)	0.512 (1)	0.03 (1)*
H1w1	0.965 (2)	0.737 (4)	0.548 (2)	0.07 (1)*
H1w2	0.901 (4)	0.909 (2)	0.544 (1)	0.08 (1)*
H1n1	0.6124	0.7498	0.6295	0.045*
H1n2	0.6894	0.5785	0.6408	0.045*
H1n3	0.7612	0.7221	0.6109	0.045*
H2n1	1.4206	0.7253	0.9165	0.037*
H2n2	1.2624	0.7107	0.9228	0.037*
H2n3	1.3280	0.8865	0.9087	0.037*
H1a	0.6899	0.7611	0.7154	0.046*
H1b	0.7697	0.9218	0.6820	0.046*
H2a	0.9857	0.7272	0.6724	0.045*
H2b	0.9057	0.5645	0.7051	0.045*
H3a	0.8990	0.7681	0.7802	0.050*
H3b	0.9845	0.9253	0.7475	0.050*
H4a	1.1207	0.5688	0.7720	0.045*
H4b	1.2052	0.7439	0.7464	0.045*
H5a	1.1644	0.9202	0.8258	0.045*
H5b	1.0867	0.7407	0.8513	0.045*
H6a	1.3258	0.5773	0.8429	0.036*
H6b	1.3981	0.7747	0.8271	0.036*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.0163 (3)	0.0102 (2)	0.0205 (3)	0.0004 (2)	−0.0015 (2)	0.0000 (2)
Fe2	0.0147 (3)	0.0104 (2)	0.0233 (3)	−0.0002 (2)	−0.0021 (2)	0.0002 (2)
S1	0.0191 (3)	0.0163 (3)	0.0234 (3)	0.0009 (3)	0.0026 (2)	0.0003 (2)
S2	0.0192 (3)	0.0153 (3)	0.0263 (3)	0.0005 (2)	−0.0087 (3)	−0.0002 (2)
O1	0.045 (1)	0.018 (1)	0.027 (1)	0.009 (1)	0.013 (1)	0.004 (1)
O2	0.020 (1)	0.017 (1)	0.029 (1)	0.002 (1)	0.005 (1)	0.004 (1)
O3	0.019 (1)	0.041 (1)	0.057 (1)	−0.004 (1)	0.006 (1)	0.017 (1)
O4	0.051 (1)	0.033 (1)	0.027 (1)	0.001 (1)	−0.006 (1)	−0.004 (1)
O5	0.023 (1)	0.016 (1)	0.027 (1)	−0.003 (1)	−0.007 (1)	0.001 (1)
O6	0.023 (1)	0.017 (1)	0.038 (1)	−0.002 (1)	−0.012 (1)	0.005 (1)
O7	0.064 (2)	0.034 (1)	0.026 (1)	−0.010 (1)	−0.015 (1)	−0.005 (1)
O8	0.017 (1)	0.027 (1)	0.066 (1)	0.002 (1)	−0.006 (1)	−0.006 (1)
O9	0.014 (1)	0.012 (1)	0.029 (1)	0.000 (1)	−0.005 (1)	0.000 (1)
O1w	0.024 (1)	0.026 (1)	0.080 (2)	0.001 (1)	−0.012 (1)	−0.004 (1)
N1	0.042 (2)	0.034 (1)	0.037 (1)	0.003 (1)	−0.012 (1)	−0.005 (1)
N2	0.027 (1)	0.036 (1)	0.030 (1)	0.007 (1)	−0.007 (1)	0.000 (1)
C1	0.041 (2)	0.039 (2)	0.034 (2)	0.004 (1)	−0.012 (1)	−0.010 (1)
C2	0.036 (2)	0.046 (2)	0.030 (2)	0.003 (1)	−0.008 (1)	−0.007 (1)
C3	0.041 (2)	0.053 (2)	0.031 (2)	0.006 (2)	−0.010 (1)	−0.010 (1)
C4	0.039 (2)	0.043 (2)	0.031 (2)	0.003 (1)	−0.004 (1)	−0.004 (1)
C5	0.037 (2)	0.042 (2)	0.034 (2)	0.008 (1)	−0.009 (1)	−0.006 (1)
C6	0.028 (2)	0.032 (2)	0.029 (2)	−0.002 (1)	−0.001 (1)	−0.002 (1)

Geometric parameters (Å, º)

Fe1—O1	2.008 (2)	C3—C4	1.527 (4)
Fe1—O1^i	2.008 (2)	C4—C5	1.517 (4)
Fe1—O6	2.003 (2)	C5—C6	1.508 (4)
Fe1—O6^i	2.003 (2)	O9—H9o	0.83 (1)
Fe1—O9	1.962 (2)	O1w—H1w1	0.84 (1)
Fe1—O9^i	1.962 (2)	O1w—H1w2	0.84 (1)
Fe2—O2	2.030 (2)	N1—H1n1	0.86
Fe2—O2^ii	2.030 (2)	N1—H1n2	0.86
Fe2—O5	2.031 (2)	N1—H1n3	0.86
Fe2—O5^ii	2.031 (2)	N2—H2n1	0.86
Fe2—O9	1.959 (2)	N2—H2n2	0.86
Fe2—O9^ii	1.959 (2)	N2—H2n3	0.86
S1—O1	1.492 (2)	C1—H1a	0.97
S1—O2	1.498 (2)	C1—H1b	0.97
S1—O3	1.448 (2)	C2—H2a	0.97
S1—O4	1.440 (2)	C2—H2b	0.97
S2—O7	1.449 (2)	C3—H3a	0.97
S2—O8	1.457 (2)	C3—H3b	0.97
S2—O5	1.491 (2)	C4—H4a	0.97
S2—O6	1.481 (2)	C4—H4b	0.97
N1—C1	1.477 (3)	C5—H5a	0.97
N2—C6	1.490 (3)	C5—H5b	0.97
C1—C2	1.514 (4)	C6—H6a	0.97
C2—C3	1.514 (4)	C6—H6b	0.97
O1—Fe1—O1^i	180	C2—C3—C4	114.3 (3)
O1—Fe1—O6	90.98 (7)	C5—C4—C3	110.4 (2)
O1—Fe1—O6^i	89.02 (7)	C6—C5—C4	113.8 (2)
O1—Fe1—O9	89.58 (7)	N2—C6—C5	110.0 (2)
O1—Fe1—O9^i	90.42 (7)	Fe2—O9—H9o	113 (2)
O1^i—Fe1—O6	89.02 (7)	Fe1—O9—H9o	114 (2)
O1^i—Fe1—O6^i	90.98 (7)	H1w1—O1w—H1w2	105 (3)
O1^i—Fe1—O9	90.42 (7)	C1—N1—H1n1	109.5
O1^i—Fe1—O9^i	89.58 (7)	C1—N1—H1n2	109.5
O6—Fe1—O6^i	180	H1n1—N1—H1n2	109.5
O6—Fe1—O9	92.32 (7)	C1—N1—H1n3	109.5
O6—Fe1—O9^i	87.68 (7)	H1n1—N1—H1n3	109.5
O6^i—Fe1—O9	87.68 (7)	H1n2—N1—H1n3	109.5
O9^i—Fe1—O6^i	92.32 (7)	C6—N2—H2n1	109.5
O9—Fe1—O9^i	180	C6—N2—H2n2	109.5
O2—Fe2—O2^ii	180	H2n1—N2—H2n2	109.5
O2—Fe2—O5	90.43 (7)	C6—N2—H2n3	109.5
O2—Fe2—O5^ii	89.57 (6)	H2n1—N2—H2n3	109.5
O2—Fe2—O9	92.79 (7)	H2n2—N2—H2n3	109.5
O2—Fe2—O9^ii	87.21 (7)	N1—C1—H1a	109.3
O2^ii—Fe2—O5	89.57 (6)	C2—C1—H1a	109.3
O2^ii—Fe2—O5^ii	90.43 (7)	N1—C1—H1b	109.3
O2^ii—Fe2—O9	87.20 (7)	C2—C1—H1b	109.3
O2^ii—Fe2—O9^ii	92.79 (7)	H1a—C1—H1b	107.9
O5—Fe2—O5^ii	180	C1—C2—H2a	109.5
O5—Fe2—O9	88.95 (7)	C3—C2—H2a	109.5
O5—Fe2—O9^ii	91.05 (7)	C1—C2—H2b	109.5
O5^ii—Fe2—O9	91.05 (7)	C3—C2—H2b	109.5
O5^ii—Fe2—O9^ii	88.95 (7)	H2a—C2—H2b	108.1
O9—Fe2—O9^ii	180	C2—C3—H3a	108.7
O4—S1—O3	112.5 (1)	C4—C3—H3a	108.7
O4—S1—O1	107.9 (1)	C2—C3—H3b	108.7
O3—S1—O1	108.6 (1)	C4—C3—H3b	108.7
O4—S1—O2	109.8 (1)	H3a—C3—H3b	107.6
O3—S1—O2	109.0 (1)	C5—C4—H4a	109.6
O1—S1—O2	108.9 (1)	C3—C4—H4a	109.6
O7—S2—O8	111.5 (1)	C5—C4—H4b	109.6
O7—S2—O6	109.6 (1)	C3—C4—H4b	109.6
O8—S2—O6	108.4 (1)	H4a—C4—H4b	108.1
O7—S2—O5	109.8 (1)	C6—C5—H5a	108.8
O8—S2—O5	108.7 (1)	C4—C5—H5a	108.8
O6—S2—O5	108.9 (1)	C6—C5—H5b	108.8
S1—O1—Fe1	135.2 (1)	C4—C5—H5b	108.8
S1—O2—Fe2	135.7 (1)	H5a—C5—H5b	107.7
S2—O5—Fe2	130.5 (1)	N2—C6—H6a	109.7
S2—O6—Fe1	141.8 (1)	C5—C6—H6a	109.7
Fe2—O9—Fe1	126.29 (9)	N2—C6—H6b	109.7
N1—C1—C2	111.7 (2)	C5—C6—H6b	109.7
C1—C2—C3	110.8 (2)	H6a—C6—H6b	108.2
O4—S1—O1—Fe1	−128.7 (2)	O7—S2—O6—Fe1	108.4 (2)
O3—S1—O1—Fe1	109.0 (2)	O8—S2—O6—Fe1	−129.8 (2)
O2—S1—O1—Fe1	−9.6 (2)	O5—S2—O6—Fe1	−11.7 (2)
O9^i—Fe1—O1—S1	−133.0 (2)	O9^i—Fe1—O6—S2	−169.6 (2)
O9—Fe1—O1—S1	47.0 (2)	O9—Fe1—O6—S2	10.4 (2)
O6^i—Fe1—O1—S1	134.7 (2)	O1—Fe1—O6—S2	100.0 (2)
O6—Fe1—O1—S1	−45.3 (2)	O1^i—Fe1—O6—S2	−80.0 (2)
O4—S1—O2—Fe2	80.2 (2)	O2—Fe2—O9—Fe1	33.6 (1)
O3—S1—O2—Fe2	−156.2 (2)	O2^ii—Fe2—O9—Fe1	−146.4 (1)
O1—S1—O2—Fe2	−37.8 (2)	O5^ii—Fe2—O9—Fe1	123.2 (1)
O9^ii—Fe2—O2—S1	−154.6 (2)	O5—Fe2—O9—Fe1	−56.8 (1)
O9—Fe2—O2—S1	25.4 (2)	O6^i—Fe1—O9—Fe2	−145.2 (1)
O5^ii—Fe2—O2—S1	−65.7 (2)	O6—Fe1—O9—Fe2	34.9 (1)
O5—Fe2—O2—S1	114.3 (2)	O1—Fe1—O9—Fe2	−56.1 (1)
O7—S2—O5—Fe2	−153.5 (1)	O1^i—Fe1—O9—Fe2	123.9 (1)
O8—S2—O5—Fe2	84.3 (2)	N1—C1—C2—C3	−179.2 (3)
O6—S2—O5—Fe2	−33.5 (2)	C1—C2—C3—C4	177.7 (3)
O9^ii—Fe2—O5—S2	−120.1 (1)	C2—C3—C4—C5	−172.0 (3)
O9—Fe2—O5—S2	60.0 (1)	C3—C4—C5—C6	−177.6 (3)
O2—Fe2—O5—S2	−32.8 (1)	C4—C5—C6—N2	−169.9 (2)
O2^ii—Fe2—O5—S2	147.2 (1)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O9—H9o···O1w	0.83 (1)	1.91 (1)	2.726 (3)	172 (2)
O1w—H1w1···O3^iii	0.84 (1)	2.07 (2)	2.826 (3)	150 (3)
O1w—H1w2···O8^ii	0.84 (1)	1.93 (2)	2.740 (3)	162 (4)
N1—H1n1···O4	0.86	2.04	2.848 (3)	157
N1—H1n2···O7^i	0.86	2.09	2.902 (3)	157
N1—H1n3···O1w	0.86	2.06	2.916 (4)	171
N2—H2n1···O8^iv	0.86	1.92	2.767 (3)	170
N2—H2n2···O9^v	0.86	2.37	3.107 (3)	143
N2—H2n3···O3^vi	0.86	2.18	3.028 (3)	169

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