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In the crystal structure of the polymeric title compound, {(C4H12N2)[Fe(OH)(SO4)2]·2H2O}n, the anion exists as a linear chain whose two independent FeIII atoms both occupy special positions of \overline{1} 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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805023408/is6107sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805023408/is6107Isup2.hkl
Contains datablock I

CCDC reference: 282525

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](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

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[piperazinium(2+) [ferrate(III)-µ-hydroxo-κ2O:O-di-µ-sulfato-κ4O:O'] dihydrate] top
Crystal data top
(C4H12N2)[Fe(OH)(SO4)2]·2H2OZ = 2
Mr = 389.17F(000) = 402
Triclinic, P1Dx = 1.972 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.0983 (6) ÅCell parameters from 1907 reflections
b = 10.4690 (9) Åθ = 2.3–28.1°
c = 10.5212 (9) ŵ = 1.53 mm1
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 tube2047 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.017
φ and ω scansθmax = 25.0°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 68
Tmin = 0.493, Tmax = 0.901k = 1211
3388 measured reflectionsl = 1212
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.134H-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 parametersΔρmax = 0.71 e Å3
0 restraintsΔρmin = 0.69 e Å3
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
xyzUiso*/UeqOcc. (<1)
Fe10.50000.50000.50000.0138 (2)
Fe21.00000.50000.50000.0134 (2)
S10.3326 (1)0.2218 (1)0.5273 (1)0.0170 (3)
S20.8403 (1)0.5584 (1)0.2085 (1)0.0176 (3)
O10.4906 (4)0.3049 (3)0.5057 (4)0.0287 (7)
O20.3231 (4)0.2267 (3)0.3878 (3)0.0299 (7)
O30.3717 (4)0.0700 (3)0.6401 (3)0.0308 (7)
O40.1423 (3)0.2910 (3)0.5770 (3)0.0203 (6)
O50.6466 (4)0.5793 (3)0.2923 (3)0.0242 (6)
O60.9945 (4)0.5082 (3)0.3039 (3)0.0234 (6)
O70.8455 (4)0.4448 (3)0.1653 (3)0.0325 (7)
O80.8756 (4)0.6980 (3)0.0792 (3)0.0353 (7)
O90.7493 (3)0.4206 (3)0.5782 (3)0.0167 (5)
O1w0.7022 (7)0.1343 (4)0.7974 (4)0.070 (1)
O2w0.670 (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
N10.1837 (5)0.0202 (4)0.4155 (4)0.0296 (8)
N20.3198 (5)0.4486 (4)0.0878 (4)0.0311 (8)
C10.1276 (6)0.1382 (5)0.5681 (5)0.035 (1)
C20.0110 (6)0.0699 (5)0.6574 (5)0.033 (1)
C30.3776 (6)0.5824 (5)0.0736 (5)0.034 (1)
C40.5068 (6)0.6579 (5)0.0730 (5)0.035 (1)
H9o0.74910.33950.65810.020*
H1w10.78430.08740.85860.084*
H1w20.58570.12890.84610.084*
H2w10.68140.01341.13830.072*0.50
H2w20.77250.11241.08240.072*0.50
H2w30.75310.00621.12670.100*0.50
H2w40.82860.11881.10890.100*0.50
H110.25350.03900.41970.035*
H120.25990.06270.36160.035*
H210.24540.47550.01770.037*
H220.24740.40340.17630.037*
H1a0.24360.19060.61530.042*
H1b0.06540.20890.56350.042*
H2a0.05320.14800.75400.039*
H2b0.05680.00800.67130.039*
H3a0.44800.55500.15410.040*
H3b0.26180.65060.07930.040*
H4a0.43230.69420.15360.042*
H4b0.55050.74210.07860.042*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0075 (4)0.0190 (4)0.0189 (4)0.0030 (3)0.0007 (3)0.0119 (3)
Fe20.0071 (4)0.0198 (4)0.0171 (4)0.0022 (3)0.0009 (3)0.0116 (3)
S10.0121 (5)0.0171 (5)0.0252 (5)0.0023 (3)0.0017 (4)0.0127 (4)
S20.0123 (5)0.0271 (5)0.0156 (5)0.0039 (4)0.0003 (4)0.0117 (4)
O10.011 (1)0.031 (2)0.057 (2)0.006 (1)0.002 (1)0.033 (2)
O20.028 (2)0.039 (2)0.033 (2)0.006 (1)0.001 (1)0.027 (1)
O30.024 (2)0.021 (2)0.040 (2)0.002 (1)0.004 (1)0.010 (1)
O40.009 (1)0.024 (1)0.030 (1)0.003 (1)0.000 (1)0.015 (1)
O50.011 (1)0.042 (2)0.020 (1)0.003 (1)0.000 (1)0.016 (1)
O60.012 (1)0.042 (2)0.023 (1)0.001 (1)0.001 (1)0.022 (1)
O70.033 (2)0.041 (2)0.035 (2)0.001 (1)0.012 (1)0.025 (1)
O80.033 (2)0.033 (2)0.025 (2)0.009 (1)0.000 (1)0.002 (1)
O90.011 (1)0.020 (1)0.018 (1)0.005 (1)0.003 (1)0.007 (1)
O1w0.121 (4)0.041 (2)0.036 (2)0.006 (2)0.006 (2)0.013 (2)
O2w0.091 (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)
N10.020 (2)0.030 (2)0.043 (2)0.004 (1)0.001 (2)0.022 (2)
N20.017 (2)0.056 (2)0.024 (2)0.011 (2)0.004 (1)0.023 (2)
C10.022 (2)0.032 (2)0.049 (3)0.002 (2)0.000 (2)0.020 (2)
C20.023 (2)0.041 (3)0.038 (2)0.009 (2)0.002 (2)0.021 (2)
C30.018 (2)0.060 (3)0.034 (2)0.008 (2)0.0001 (2)0.031 (2)
C40.023 (2)0.044 (3)0.033 (2)0.004 (2)0.001 (2)0.015 (2)
Geometric parameters (Å, º) top
Fe1—O12.030 (3)N2—C4vi1.496 (6)
Fe1—O1i2.030 (3)C1—C21.508 (6)
Fe1—O52.025 (2)C2—N1v1.474 (5)
Fe1—O5i2.025 (2)C3—C41.522 (6)
Fe1—O91.956 (2)C4—N2vi1.496 (6)
Fe1—O9i1.956 (2)O9—H9o0.8500
Fe2—O4ii2.021 (2)O1w—H1w10.85
Fe2—O4i2.021 (2)O1w—H1w20.86
Fe2—O62.032 (2)O2w—H2w10.86
Fe2—O6iii2.032 (2)O2w—H2w20.86
Fe2—O91.964 (2)O2w'—H2w30.87
Fe2—O9iii1.964 (2)O2w'—H2w40.87
S1—O31.449 (3)N1—H110.90
S1—O21.460 (3)N1—H120.90
S1—O11.483 (3)N2—H210.90
S1—O41.491 (2)N2—H220.90
S2—O81.448 (3)C1—H1a0.97
S2—O71.459 (3)C1—H1b0.97
S2—O51.485 (3)C2—H2a0.97
S2—O61.486 (3)C2—H2b0.97
O4—Fe2iv2.021 (2)C3—H3a0.97
N1—C2v1.474 (5)C3—H3b0.97
N1—C11.494 (6)C4—H4a0.97
N2—C31.476 (6)C4—H4b0.97
O1—Fe1—O1i180H2w1—O2w—H2w2109.2
O1—Fe1—O591.7 (1)H2w3—O2w'—H2w4105.0
O1—Fe1—O5i88.4 (1)C2v—N1—C1111.8 (3)
O1—Fe1—O990.4 (1)C2v—N1—H11109.3
O1—Fe1—O9i89.6 (1)C1—N1—H11109.3
O5—Fe1—O5i180C2v—N1—H12109.3
O5—Fe1—O989.6 (1)C1—N1—H12109.3
O5—Fe1—O9i90.4 (1)H11—N1—H12107.9
O9—Fe1—O9i180C3—N2—C4vi112.0 (3)
O4ii—Fe2—O4i180C3—N2—H21109.2
O4ii—Fe2—O691.2 (1)C4vi—N2—H21109.2
O4ii—Fe2—O6iii88.8 (1)C3—N2—H22109.2
O4ii—Fe2—O989.7 (1)C4vi—N2—H22109.2
O4ii—Fe2—O9iii90.3 (1)H21—N2—H22107.9
O6—Fe2—O6iii180N1—C1—C2110.0 (4)
O6—Fe2—O990.0 (1)N1—C1—H1a109.7
O6—Fe2—O9iii90.0 (1)C2—C1—H1a109.7
O9—Fe2—O9iii180N1—C1—H1b109.7
O3—S1—O2110.6 (2)C2—C1—H1b109.7
O3—S1—O1109.4 (2)H1a—C1—H1b108.2
O2—S1—O1109.2 (2)N1v—C2—C1111.7 (4)
O3—S1—O4108.7 (2)N1v—C2—H2a109.3
O2—S1—O4109.5 (2)C1—C2—H2a109.3
O1—S1—O4109.5 (2)N1v—C2—H2b109.3
O8—S2—O7110.3 (2)C1—C2—H2b109.3
O8—S2—O5108.9 (2)H2a—C2—H2b107.9
O7—S2—O5110.3 (2)N2—C3—C4110.3 (3)
O8—S2—O6109.9 (2)N2—C3—H3a109.6
O7—S2—O6108.0 (2)C4—C3—H3a109.6
O5—S2—O6109.4 (1)N2—C3—H3b109.6
S1—O1—Fe1135.0 (2)C4—C3—H3b109.6
S1—O4—Fe2iv133.9 (2)H3a—C3—H3b108.1
S2—O5—Fe1141.4 (2)N2vi—C4—C3110.3 (4)
S2—O6—Fe2133.7 (2)N2vi—C4—H4a109.6
Fe1—O9—Fe2129.7 (1)C3—C4—H4a109.6
Fe1—O9—H9o115.1N2vi—C4—H4b109.6
Fe2—O9—H9o115.1C3—C4—H4b109.6
H1w1—O1w—H1w2108.6H4a—C4—H4b108.1
O3—S1—O1—Fe1129.5 (3)O7—S2—O6—Fe2133.1 (2)
O2—S1—O1—Fe1109.4 (3)O5—S2—O6—Fe213.1 (3)
O4—S1—O1—Fe110.5 (3)O9iii—Fe2—O6—S2135.8 (2)
O9—Fe1—O1—S1149.5 (3)O9—Fe2—O6—S244.2 (2)
O9i—Fe1—O1—S130.5 (3)O4ii—Fe2—O6—S2133.9 (2)
O5—Fe1—O1—S1120.9 (3)O4i—Fe2—O6—S246.1 (2)
O5i—Fe1—O1—S159.1 (3)O5—Fe1—O9—Fe234.35 (17)
O3—S1—O4—Fe2iv171.3 (2)O5i—Fe1—O9—Fe2145.7 (2)
O2—S1—O4—Fe2iv67.8 (2)O1—Fe1—O9—Fe2126.0 (2)
O1—S1—O4—Fe2iv51.9 (3)O1i—Fe1—O9—Fe254.0 (2)
O8—S2—O5—Fe1150.8 (3)O4ii—Fe2—O9—Fe1145.9 (2)
O7—S2—O5—Fe188.0 (3)O4i—Fe2—O9—Fe134.2 (2)
O6—S2—O5—Fe130.7 (3)O6—Fe2—O9—Fe154.7 (2)
O9—Fe1—O5—S220.5 (3)O6iii—Fe2—O9—Fe1125.4 (2)
O9i—Fe1—O5—S2159.5 (3)C2v—N1—C1—C255.3 (5)
O1—Fe1—O5—S269.9 (3)N1—C1—C2—N1v55.2 (5)
O1i—Fe1—O5—S2110.1 (3)C4vi—N2—C3—C456.8 (5)
O8—S2—O6—Fe2106.5 (3)N2—C3—C4—N2vi55.8 (5)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z; (iii) x+2, y+1, z+1; (iv) x1, y, z; (v) x, y, z+1; (vi) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9o···O1w0.851.972.773 (4)158
O1w—H1w1···O2w0.852.162.657 (8)117
O1w—H1w2···O2wvii0.861.992.78 (1)152
O1w—H1w1···O2w0.852.062.83 (1)150
O2w—H2w1···O3vii0.862.062.752 (8)137
O2w—H2w2···O8viii0.861.972.717 (8)146
O2w—H2w3···O3vii0.872.202.91 (1)139
O2w—H2w4···O8viii0.872.032.82 (1)149
N1—H11···O20.901.982.835 (5)157
N1—H12···O1wix0.902.092.909 (5)151
N2—H21···O7vi0.901.892.762 (4)163
N2—H22···O20.902.172.852 (5)132
Symmetry codes: (vi) x+1, y+1, z; (vii) x+1, y, z+2; (viii) x, y1, z+1; (ix) x+1, y, z+1.
 

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