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metal-organic compounds
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.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805005350/bt6606sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805005350/bt6606Isup2.hkl |
CCDC reference: 269380
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (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 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.
catena-Poly[hexamethylenediaminium
[ferrate(III)-µ-hydroxo-κ2O:O-di-µ-sulfato-κ4O:O'] monohydrate] top
Crystal data top
(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) Å3 | 0.35 × 0.12 × 0.12 mm |
Z = 4 |
Data collection top
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 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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.100 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.99 | w = 1/[σ2(Fo2) + (0.0548P)2] where P = (Fo2 + 2Fc2)/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 (Å2) top
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 (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
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) top
Fe1—O1 | 2.008 (2) | C3—C4 | 1.527 (4) |
Fe1—O1i | 2.008 (2) | C4—C5 | 1.517 (4) |
Fe1—O6 | 2.003 (2) | C5—C6 | 1.508 (4) |
Fe1—O6i | 2.003 (2) | O9—H9o | 0.83 (1) |
Fe1—O9 | 1.962 (2) | O1w—H1w1 | 0.84 (1) |
Fe1—O9i | 1.962 (2) | O1w—H1w2 | 0.84 (1) |
Fe2—O2 | 2.030 (2) | N1—H1n1 | 0.86 |
Fe2—O2ii | 2.030 (2) | N1—H1n2 | 0.86 |
Fe2—O5 | 2.031 (2) | N1—H1n3 | 0.86 |
Fe2—O5ii | 2.031 (2) | N2—H2n1 | 0.86 |
Fe2—O9 | 1.959 (2) | N2—H2n2 | 0.86 |
Fe2—O9ii | 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—O1i | 180 | C2—C3—C4 | 114.3 (3) |
O1—Fe1—O6 | 90.98 (7) | C5—C4—C3 | 110.4 (2) |
O1—Fe1—O6i | 89.02 (7) | C6—C5—C4 | 113.8 (2) |
O1—Fe1—O9 | 89.58 (7) | N2—C6—C5 | 110.0 (2) |
O1—Fe1—O9i | 90.42 (7) | Fe2—O9—H9o | 113 (2) |
O1i—Fe1—O6 | 89.02 (7) | Fe1—O9—H9o | 114 (2) |
O1i—Fe1—O6i | 90.98 (7) | H1w1—O1w—H1w2 | 105 (3) |
O1i—Fe1—O9 | 90.42 (7) | C1—N1—H1n1 | 109.5 |
O1i—Fe1—O9i | 89.58 (7) | C1—N1—H1n2 | 109.5 |
O6—Fe1—O6i | 180 | H1n1—N1—H1n2 | 109.5 |
O6—Fe1—O9 | 92.32 (7) | C1—N1—H1n3 | 109.5 |
O6—Fe1—O9i | 87.68 (7) | H1n1—N1—H1n3 | 109.5 |
O6i—Fe1—O9 | 87.68 (7) | H1n2—N1—H1n3 | 109.5 |
O9i—Fe1—O6i | 92.32 (7) | C6—N2—H2n1 | 109.5 |
O9—Fe1—O9i | 180 | C6—N2—H2n2 | 109.5 |
O2—Fe2—O2ii | 180 | H2n1—N2—H2n2 | 109.5 |
O2—Fe2—O5 | 90.43 (7) | C6—N2—H2n3 | 109.5 |
O2—Fe2—O5ii | 89.57 (6) | H2n1—N2—H2n3 | 109.5 |
O2—Fe2—O9 | 92.79 (7) | H2n2—N2—H2n3 | 109.5 |
O2—Fe2—O9ii | 87.21 (7) | N1—C1—H1a | 109.3 |
O2ii—Fe2—O5 | 89.57 (6) | C2—C1—H1a | 109.3 |
O2ii—Fe2—O5ii | 90.43 (7) | N1—C1—H1b | 109.3 |
O2ii—Fe2—O9 | 87.20 (7) | C2—C1—H1b | 109.3 |
O2ii—Fe2—O9ii | 92.79 (7) | H1a—C1—H1b | 107.9 |
O5—Fe2—O5ii | 180 | C1—C2—H2a | 109.5 |
O5—Fe2—O9 | 88.95 (7) | C3—C2—H2a | 109.5 |
O5—Fe2—O9ii | 91.05 (7) | C1—C2—H2b | 109.5 |
O5ii—Fe2—O9 | 91.05 (7) | C3—C2—H2b | 109.5 |
O5ii—Fe2—O9ii | 88.95 (7) | H2a—C2—H2b | 108.1 |
O9—Fe2—O9ii | 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) |
O9i—Fe1—O1—S1 | −133.0 (2) | O9i—Fe1—O6—S2 | −169.6 (2) |
O9—Fe1—O1—S1 | 47.0 (2) | O9—Fe1—O6—S2 | 10.4 (2) |
O6i—Fe1—O1—S1 | 134.7 (2) | O1—Fe1—O6—S2 | 100.0 (2) |
O6—Fe1—O1—S1 | −45.3 (2) | O1i—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) | O2ii—Fe2—O9—Fe1 | −146.4 (1) |
O1—S1—O2—Fe2 | −37.8 (2) | O5ii—Fe2—O9—Fe1 | 123.2 (1) |
O9ii—Fe2—O2—S1 | −154.6 (2) | O5—Fe2—O9—Fe1 | −56.8 (1) |
O9—Fe2—O2—S1 | 25.4 (2) | O6i—Fe1—O9—Fe2 | −145.2 (1) |
O5ii—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) | O1i—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) |
O9ii—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) |
O2ii—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) top
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···O3iii | 0.84 (1) | 2.07 (2) | 2.826 (3) | 150 (3) |
O1w—H1w2···O8ii | 0.84 (1) | 1.93 (2) | 2.740 (3) | 162 (4) |
N1—H1n1···O4 | 0.86 | 2.04 | 2.848 (3) | 157 |
N1—H1n2···O7i | 0.86 | 2.09 | 2.902 (3) | 157 |
N1—H1n3···O1w | 0.86 | 2.06 | 2.916 (4) | 171 |
N2—H2n1···O8iv | 0.86 | 1.92 | 2.767 (3) | 170 |
N2—H2n2···O9v | 0.86 | 2.37 | 3.107 (3) | 143 |
N2—H2n3···O3vi | 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. |
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