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In the crystal structure of the polymeric title compound, {(C
4H
12N
2)[Fe(OH)(SO
4)
2]·2H
2O}
n, the anion exists as a linear chain whose two independent Fe
III atoms both occupy special positions of
site symmetry. The two independent cations, which also lie on inversion sites, interact with the polyanionic chain and with the uncoordinated water molecules to form a tight-held three-dimensional network.
Supporting information
CCDC reference: 282525
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.007 Å
- Disorder in main residue
- R factor = 0.035
- wR factor = 0.134
- Data-to-parameter ratio = 11.7
checkCIF/PLATON results
No syntax errors found
Alert level B
ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75
Tmin and Tmax reported: 0.493 0.901
Tmin(prime) and Tmax expected: 0.690 0.899
RR(prime) = 0.712
Please check that your absorption correction is appropriate.
PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.71
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 .... ?
PLAT301_ALERT_3_C Main Residue Disorder ......................... 1.00 Perc.
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7
PLAT432_ALERT_2_C Short Inter X...Y Contact O2 .. C4 .. 2.96 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 7
0 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
6 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
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
5 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
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[piperazinium(2+)
[ferrate(III)-µ-hydroxo-
κ2O:
O-di-µ-sulfato-
κ4O:
O'] dihydrate]
top
Crystal data top
(C4H12N2)[Fe(OH)(SO4)2]·2H2O | Z = 2 |
Mr = 389.17 | F(000) = 402 |
Triclinic, P1 | Dx = 1.972 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.0983 (6) Å | Cell parameters from 1907 reflections |
b = 10.4690 (9) Å | θ = 2.3–28.1° |
c = 10.5212 (9) Å | µ = 1.53 mm−1 |
α = 60.421 (1)° | T = 295 K |
β = 76.616 (1)° | Block, yellow |
γ = 76.797 (2)° | 0.24 × 0.09 × 0.07 mm |
V = 655.4 (1) Å3 | |
Data collection top
Bruker APEX area-detector diffractometer | 2264 independent reflections |
Radiation source: fine-focus sealed tube | 2047 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.017 |
φ and ω scans | θmax = 25.0°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −6→8 |
Tmin = 0.493, Tmax = 0.901 | k = −12→11 |
3388 measured reflections | l = −12→12 |
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) = 0.134 | H-atom parameters constrained |
S = 1.22 | w = 1/[σ2(Fo2) + (0.0823P)2 + 0.1835P] where P = (Fo2 + 2Fc2)/3 |
2264 reflections | (Δ/σ)max = 0.001 |
193 parameters | Δρmax = 0.71 e Å−3 |
0 restraints | Δρmin = −0.69 e Å−3 |
Special details top
Refinement. Although the crystal was measured to a 2θ limit of 56°, the set of reflections
was only 93% complete; consequently, the cutoff was set at 50° in the
refinement. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Fe1 | 0.5000 | 0.5000 | 0.5000 | 0.0138 (2) | |
Fe2 | 1.0000 | 0.5000 | 0.5000 | 0.0134 (2) | |
S1 | 0.3326 (1) | 0.2218 (1) | 0.5273 (1) | 0.0170 (3) | |
S2 | 0.8403 (1) | 0.5584 (1) | 0.2085 (1) | 0.0176 (3) | |
O1 | 0.4906 (4) | 0.3049 (3) | 0.5057 (4) | 0.0287 (7) | |
O2 | 0.3231 (4) | 0.2267 (3) | 0.3878 (3) | 0.0299 (7) | |
O3 | 0.3717 (4) | 0.0700 (3) | 0.6401 (3) | 0.0308 (7) | |
O4 | 0.1423 (3) | 0.2910 (3) | 0.5770 (3) | 0.0203 (6) | |
O5 | 0.6466 (4) | 0.5793 (3) | 0.2923 (3) | 0.0242 (6) | |
O6 | 0.9945 (4) | 0.5082 (3) | 0.3039 (3) | 0.0234 (6) | |
O7 | 0.8455 (4) | 0.4448 (3) | 0.1653 (3) | 0.0325 (7) | |
O8 | 0.8756 (4) | 0.6980 (3) | 0.0792 (3) | 0.0353 (7) | |
O9 | 0.7493 (3) | 0.4206 (3) | 0.5782 (3) | 0.0167 (5) | |
O1w | 0.7022 (7) | 0.1343 (4) | 0.7974 (4) | 0.070 (1) | |
O2w | 0.670 (1) | −0.0514 (8) | 1.0849 (8) | 0.060 (2) | 0.50 |
O2w' | 0.842 (2) | −0.026 (1) | 1.073 (1) | 0.083 (3) | 0.50 |
N1 | 0.1837 (5) | −0.0202 (4) | 0.4155 (4) | 0.0296 (8) | |
N2 | 0.3198 (5) | 0.4486 (4) | 0.0878 (4) | 0.0311 (8) | |
C1 | 0.1276 (6) | −0.1382 (5) | 0.5681 (5) | 0.035 (1) | |
C2 | −0.0110 (6) | −0.0699 (5) | 0.6574 (5) | 0.033 (1) | |
C3 | 0.3776 (6) | 0.5824 (5) | 0.0736 (5) | 0.034 (1) | |
C4 | 0.5068 (6) | 0.6579 (5) | −0.0730 (5) | 0.035 (1) | |
H9o | 0.7491 | 0.3395 | 0.6581 | 0.020* | |
H1w1 | 0.7843 | 0.0874 | 0.8586 | 0.084* | |
H1w2 | 0.5857 | 0.1289 | 0.8461 | 0.084* | |
H2w1 | 0.6814 | −0.0134 | 1.1383 | 0.072* | 0.50 |
H2w2 | 0.7725 | −0.1124 | 1.0824 | 0.072* | 0.50 |
H2w3 | 0.7531 | 0.0062 | 1.1267 | 0.100* | 0.50 |
H2w4 | 0.8286 | −0.1188 | 1.1089 | 0.100* | 0.50 |
H11 | 0.2535 | 0.0390 | 0.4197 | 0.035* | |
H12 | 0.2599 | −0.0627 | 0.3616 | 0.035* | |
H21 | 0.2454 | 0.4755 | 0.0177 | 0.037* | |
H22 | 0.2474 | 0.4034 | 0.1763 | 0.037* | |
H1a | 0.2436 | −0.1906 | 0.6153 | 0.042* | |
H1b | 0.0654 | −0.2089 | 0.5635 | 0.042* | |
H2a | −0.0532 | −0.1480 | 0.7540 | 0.039* | |
H2b | 0.0568 | −0.0080 | 0.6713 | 0.039* | |
H3a | 0.4480 | 0.5550 | 0.1541 | 0.040* | |
H3b | 0.2618 | 0.6506 | 0.0793 | 0.040* | |
H4a | 0.4323 | 0.6942 | −0.1536 | 0.042* | |
H4b | 0.5505 | 0.7421 | −0.0786 | 0.042* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0075 (4) | 0.0190 (4) | 0.0189 (4) | −0.0030 (3) | −0.0007 (3) | −0.0119 (3) |
Fe2 | 0.0071 (4) | 0.0198 (4) | 0.0171 (4) | −0.0022 (3) | −0.0009 (3) | −0.0116 (3) |
S1 | 0.0121 (5) | 0.0171 (5) | 0.0252 (5) | −0.0023 (3) | −0.0017 (4) | −0.0127 (4) |
S2 | 0.0123 (5) | 0.0271 (5) | 0.0156 (5) | −0.0039 (4) | −0.0003 (4) | −0.0117 (4) |
O1 | 0.011 (1) | 0.031 (2) | 0.057 (2) | −0.006 (1) | 0.002 (1) | −0.033 (2) |
O2 | 0.028 (2) | 0.039 (2) | 0.033 (2) | −0.006 (1) | 0.001 (1) | −0.027 (1) |
O3 | 0.024 (2) | 0.021 (2) | 0.040 (2) | 0.002 (1) | −0.004 (1) | −0.010 (1) |
O4 | 0.009 (1) | 0.024 (1) | 0.030 (1) | −0.003 (1) | 0.000 (1) | −0.015 (1) |
O5 | 0.011 (1) | 0.042 (2) | 0.020 (1) | −0.003 (1) | 0.000 (1) | −0.016 (1) |
O6 | 0.012 (1) | 0.042 (2) | 0.023 (1) | −0.001 (1) | −0.001 (1) | −0.022 (1) |
O7 | 0.033 (2) | 0.041 (2) | 0.035 (2) | 0.001 (1) | −0.012 (1) | −0.025 (1) |
O8 | 0.033 (2) | 0.033 (2) | 0.025 (2) | −0.009 (1) | 0.000 (1) | −0.002 (1) |
O9 | 0.011 (1) | 0.020 (1) | 0.018 (1) | −0.005 (1) | −0.003 (1) | −0.007 (1) |
O1w | 0.121 (4) | 0.041 (2) | 0.036 (2) | −0.006 (2) | −0.006 (2) | −0.013 (2) |
O2w | 0.091 (7) | 0.033 (4) | 0.033 (4) | 0.012 (4) | −0.015 (4) | −0.004 (3) |
O2w' | 0.13 (1) | 0.062 (6) | 0.044 (5) | −0.028 (6) | −0.001 (6) | −0.013 (4) |
N1 | 0.020 (2) | 0.030 (2) | 0.043 (2) | −0.004 (1) | 0.001 (2) | −0.022 (2) |
N2 | 0.017 (2) | 0.056 (2) | 0.024 (2) | −0.011 (2) | 0.004 (1) | −0.023 (2) |
C1 | 0.022 (2) | 0.032 (2) | 0.049 (3) | −0.002 (2) | 0.000 (2) | −0.020 (2) |
C2 | 0.023 (2) | 0.041 (3) | 0.038 (2) | −0.009 (2) | −0.002 (2) | −0.021 (2) |
C3 | 0.018 (2) | 0.060 (3) | 0.034 (2) | −0.008 (2) | 0.0001 (2) | −0.031 (2) |
C4 | 0.023 (2) | 0.044 (3) | 0.033 (2) | −0.004 (2) | −0.001 (2) | −0.015 (2) |
Geometric parameters (Å, º) top
Fe1—O1 | 2.030 (3) | N2—C4vi | 1.496 (6) |
Fe1—O1i | 2.030 (3) | C1—C2 | 1.508 (6) |
Fe1—O5 | 2.025 (2) | C2—N1v | 1.474 (5) |
Fe1—O5i | 2.025 (2) | C3—C4 | 1.522 (6) |
Fe1—O9 | 1.956 (2) | C4—N2vi | 1.496 (6) |
Fe1—O9i | 1.956 (2) | O9—H9o | 0.8500 |
Fe2—O4ii | 2.021 (2) | O1w—H1w1 | 0.85 |
Fe2—O4i | 2.021 (2) | O1w—H1w2 | 0.86 |
Fe2—O6 | 2.032 (2) | O2w—H2w1 | 0.86 |
Fe2—O6iii | 2.032 (2) | O2w—H2w2 | 0.86 |
Fe2—O9 | 1.964 (2) | O2w'—H2w3 | 0.87 |
Fe2—O9iii | 1.964 (2) | O2w'—H2w4 | 0.87 |
S1—O3 | 1.449 (3) | N1—H11 | 0.90 |
S1—O2 | 1.460 (3) | N1—H12 | 0.90 |
S1—O1 | 1.483 (3) | N2—H21 | 0.90 |
S1—O4 | 1.491 (2) | N2—H22 | 0.90 |
S2—O8 | 1.448 (3) | C1—H1a | 0.97 |
S2—O7 | 1.459 (3) | C1—H1b | 0.97 |
S2—O5 | 1.485 (3) | C2—H2a | 0.97 |
S2—O6 | 1.486 (3) | C2—H2b | 0.97 |
O4—Fe2iv | 2.021 (2) | C3—H3a | 0.97 |
N1—C2v | 1.474 (5) | C3—H3b | 0.97 |
N1—C1 | 1.494 (6) | C4—H4a | 0.97 |
N2—C3 | 1.476 (6) | C4—H4b | 0.97 |
| | | |
O1—Fe1—O1i | 180 | H2w1—O2w—H2w2 | 109.2 |
O1—Fe1—O5 | 91.7 (1) | H2w3—O2w'—H2w4 | 105.0 |
O1—Fe1—O5i | 88.4 (1) | C2v—N1—C1 | 111.8 (3) |
O1—Fe1—O9 | 90.4 (1) | C2v—N1—H11 | 109.3 |
O1—Fe1—O9i | 89.6 (1) | C1—N1—H11 | 109.3 |
O5—Fe1—O5i | 180 | C2v—N1—H12 | 109.3 |
O5—Fe1—O9 | 89.6 (1) | C1—N1—H12 | 109.3 |
O5—Fe1—O9i | 90.4 (1) | H11—N1—H12 | 107.9 |
O9—Fe1—O9i | 180 | C3—N2—C4vi | 112.0 (3) |
O4ii—Fe2—O4i | 180 | C3—N2—H21 | 109.2 |
O4ii—Fe2—O6 | 91.2 (1) | C4vi—N2—H21 | 109.2 |
O4ii—Fe2—O6iii | 88.8 (1) | C3—N2—H22 | 109.2 |
O4ii—Fe2—O9 | 89.7 (1) | C4vi—N2—H22 | 109.2 |
O4ii—Fe2—O9iii | 90.3 (1) | H21—N2—H22 | 107.9 |
O6—Fe2—O6iii | 180 | N1—C1—C2 | 110.0 (4) |
O6—Fe2—O9 | 90.0 (1) | N1—C1—H1a | 109.7 |
O6—Fe2—O9iii | 90.0 (1) | C2—C1—H1a | 109.7 |
O9—Fe2—O9iii | 180 | N1—C1—H1b | 109.7 |
O3—S1—O2 | 110.6 (2) | C2—C1—H1b | 109.7 |
O3—S1—O1 | 109.4 (2) | H1a—C1—H1b | 108.2 |
O2—S1—O1 | 109.2 (2) | N1v—C2—C1 | 111.7 (4) |
O3—S1—O4 | 108.7 (2) | N1v—C2—H2a | 109.3 |
O2—S1—O4 | 109.5 (2) | C1—C2—H2a | 109.3 |
O1—S1—O4 | 109.5 (2) | N1v—C2—H2b | 109.3 |
O8—S2—O7 | 110.3 (2) | C1—C2—H2b | 109.3 |
O8—S2—O5 | 108.9 (2) | H2a—C2—H2b | 107.9 |
O7—S2—O5 | 110.3 (2) | N2—C3—C4 | 110.3 (3) |
O8—S2—O6 | 109.9 (2) | N2—C3—H3a | 109.6 |
O7—S2—O6 | 108.0 (2) | C4—C3—H3a | 109.6 |
O5—S2—O6 | 109.4 (1) | N2—C3—H3b | 109.6 |
S1—O1—Fe1 | 135.0 (2) | C4—C3—H3b | 109.6 |
S1—O4—Fe2iv | 133.9 (2) | H3a—C3—H3b | 108.1 |
S2—O5—Fe1 | 141.4 (2) | N2vi—C4—C3 | 110.3 (4) |
S2—O6—Fe2 | 133.7 (2) | N2vi—C4—H4a | 109.6 |
Fe1—O9—Fe2 | 129.7 (1) | C3—C4—H4a | 109.6 |
Fe1—O9—H9o | 115.1 | N2vi—C4—H4b | 109.6 |
Fe2—O9—H9o | 115.1 | C3—C4—H4b | 109.6 |
H1w1—O1w—H1w2 | 108.6 | H4a—C4—H4b | 108.1 |
| | | |
O3—S1—O1—Fe1 | −129.5 (3) | O7—S2—O6—Fe2 | −133.1 (2) |
O2—S1—O1—Fe1 | 109.4 (3) | O5—S2—O6—Fe2 | −13.1 (3) |
O4—S1—O1—Fe1 | −10.5 (3) | O9iii—Fe2—O6—S2 | −135.8 (2) |
O9—Fe1—O1—S1 | 149.5 (3) | O9—Fe2—O6—S2 | 44.2 (2) |
O9i—Fe1—O1—S1 | −30.5 (3) | O4ii—Fe2—O6—S2 | 133.9 (2) |
O5—Fe1—O1—S1 | −120.9 (3) | O4i—Fe2—O6—S2 | −46.1 (2) |
O5i—Fe1—O1—S1 | 59.1 (3) | O5—Fe1—O9—Fe2 | 34.35 (17) |
O3—S1—O4—Fe2iv | 171.3 (2) | O5i—Fe1—O9—Fe2 | −145.7 (2) |
O2—S1—O4—Fe2iv | −67.8 (2) | O1—Fe1—O9—Fe2 | 126.0 (2) |
O1—S1—O4—Fe2iv | 51.9 (3) | O1i—Fe1—O9—Fe2 | −54.0 (2) |
O8—S2—O5—Fe1 | −150.8 (3) | O4ii—Fe2—O9—Fe1 | −145.9 (2) |
O7—S2—O5—Fe1 | 88.0 (3) | O4i—Fe2—O9—Fe1 | 34.2 (2) |
O6—S2—O5—Fe1 | −30.7 (3) | O6—Fe2—O9—Fe1 | −54.7 (2) |
O9—Fe1—O5—S2 | 20.5 (3) | O6iii—Fe2—O9—Fe1 | 125.4 (2) |
O9i—Fe1—O5—S2 | −159.5 (3) | C2v—N1—C1—C2 | −55.3 (5) |
O1—Fe1—O5—S2 | −69.9 (3) | N1—C1—C2—N1v | 55.2 (5) |
O1i—Fe1—O5—S2 | 110.1 (3) | C4vi—N2—C3—C4 | 56.8 (5) |
O8—S2—O6—Fe2 | 106.5 (3) | N2—C3—C4—N2vi | −55.8 (5) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1, y, z; (iii) −x+2, −y+1, −z+1; (iv) x−1, y, z; (v) −x, −y, −z+1; (vi) −x+1, −y+1, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O9—H9o···O1w | 0.85 | 1.97 | 2.773 (4) | 158 |
O1w—H1w1···O2w | 0.85 | 2.16 | 2.657 (8) | 117 |
O1w—H1w2···O2wvii | 0.86 | 1.99 | 2.78 (1) | 152 |
O1w—H1w1···O2w′ | 0.85 | 2.06 | 2.83 (1) | 150 |
O2w—H2w1···O3vii | 0.86 | 2.06 | 2.752 (8) | 137 |
O2w—H2w2···O8viii | 0.86 | 1.97 | 2.717 (8) | 146 |
O2w′—H2w3···O3vii | 0.87 | 2.20 | 2.91 (1) | 139 |
O2w′—H2w4···O8viii | 0.87 | 2.03 | 2.82 (1) | 149 |
N1—H11···O2 | 0.90 | 1.98 | 2.835 (5) | 157 |
N1—H12···O1wix | 0.90 | 2.09 | 2.909 (5) | 151 |
N2—H21···O7vi | 0.90 | 1.89 | 2.762 (4) | 163 |
N2—H22···O2 | 0.90 | 2.17 | 2.852 (5) | 132 |
Symmetry codes: (vi) −x+1, −y+1, −z; (vii) −x+1, −y, −z+2; (viii) x, y−1, z+1; (ix) −x+1, −y, −z+1. |
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