The reaction of ferric sulfate with ethylenediamine in the presence of acid under hydrothermal conditions results in the title compound, (C
2H
10N
2)
2[Fe
III(OH)(SO
4)
2](SO
4)·H
2O. The six-coordinate ferrate dianion participates in a μ
2-hydroxo-di-μ
2-sulfate-bridged chain. The component species interact with each other by an extensive network of O—H
O and N—H
O hydrogen bonds. The two independent Fe
III atoms lie on sites of
symmetry.
Supporting information
CCDC reference: 282365
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.003 Å
- R factor = 0.028
- wR factor = 0.081
- Data-to-parameter ratio = 11.2
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 8
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 14
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.840(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
N1 -H1N1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.96(3), Rep 0.950(10) ...... 3.00 su-Rat
C1 -H1A 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.840(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
N1 -H3# 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.98(3), Rep 1.990(10) ...... 3.00 su-Rat
H2# -O7 1.555 1.545
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
9 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
7 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
0 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
checkCIF publication errors
Alert level A
PUBL023_ALERT_1_A There is a mismatched ^ on line 131
[Fe(OH)(SO~4~)~2~]~n~ chain whose Fe^III atoms are bridged by the hydroxo and
If you require a ^ then it should be escaped
with a \, i.e. \^
Otherwise there must be a matching closing ~, e.g. ^12^C
1 ALERT level A = Data missing that is essential or data in wrong format
0 ALERT level G = General alerts. Data that may be required is missing
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[[bis(ethane-1,2-diaminium)
[ferrate(III)-µ-hydroxo-
κ2O:
O-di-µ-sulfato-
κ4O:
O']] sulfate monohydrate]
top
Crystal data top
(C2H10N2)2[Fe(OH)(SO4)2](SO4)·2H2O | Z = 2 |
Mr = 503.29 | F(000) = 522 |
Triclinic, P1 | Dx = 2.029 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.1352 (4) Å | Cell parameters from 4504 reflections |
b = 8.7869 (5) Å | θ = 2.3–28.4° |
c = 13.1860 (7) Å | µ = 1.38 mm−1 |
α = 88.659 (1)° | T = 295 K |
β = 85.782 (1)° | Plate, yellow |
γ = 88.145 (1)° | 0.25 × 0.06 × 0.04 mm |
V = 823.86 (8) Å3 | |
Data collection top
Bruker APEX area-detector diffractometer | 3695 independent reflections |
Radiation source: fine-focus sealed tube | 3324 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
φ and ω scans | θmax = 27.5°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −9→9 |
Tmin = 0.795, Tmax = 0.947 | k = −11→11 |
9220 measured reflections | l = −16→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)] = 0.028 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.081 | All H-atom parameters refined |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0499P)2 + 0.2749P] where P = (Fo2 + 2Fc2)/3 |
3695 reflections | (Δ/σ)max = 0.001 |
330 parameters | Δρmax = 0.43 e Å−3 |
23 restraints | Δρmin = −0.32 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 | 0.0130 (1) | |
Fe2 | 0.0000 | 0.5000 | 0.5000 | 0.0121 (1) | |
S1 | 0.26550 (6) | 0.55848 (5) | 0.29144 (4) | 0.01369 (12) | |
S2 | 0.23751 (6) | 0.79738 (5) | 0.54691 (4) | 0.01315 (12) | |
S3 | 0.73865 (7) | 0.85050 (6) | 0.07837 (4) | 0.01864 (13) | |
O1 | 0.4351 (2) | 0.5136 (2) | 0.3477 (1) | 0.0195 (3) | |
O2 | 0.0957 (2) | 0.4938 (2) | 0.3502 (1) | 0.0172 (3) | |
O3 | 0.2837 (2) | 0.4921 (2) | 0.1922 (1) | 0.0252 (3) | |
O4 | 0.2409 (2) | 0.7239 (2) | 0.2870 (1) | 0.0246 (3) | |
O5 | 0.4179 (2) | 0.7171 (2) | 0.5119 (1) | 0.0202 (3) | |
O6 | 0.0775 (2) | 0.7155 (2) | 0.5086 (1) | 0.0174 (3) | |
O7 | 0.2415 (2) | 0.9501 (2) | 0.5010 (1) | 0.0213 (3) | |
O8 | 0.2198 (2) | 0.8005 (2) | 0.6568 (1) | 0.0245 (3) | |
O9 | 0.2475 (2) | 0.4344 (2) | 0.5435 (1) | 0.0149 (3) | |
O10 | 0.7026 (3) | 0.8595 (2) | −0.0293 (1) | 0.0431 (5) | |
O11 | 0.9066 (2) | 0.7535 (2) | 0.0953 (1) | 0.0335 (4) | |
O12 | 0.5764 (2) | 0.7824 (2) | 0.1364 (1) | 0.0267 (4) | |
O13 | 0.7678 (2) | 1.0042 (2) | 0.1163 (1) | 0.0294 (4) | |
O1w | 0.1502 (2) | 0.1695 (2) | 0.6476 (1) | 0.0256 (3) | |
N1 | 0.5114 (3) | 0.0239 (2) | 0.6893 (2) | 0.0234 (4) | |
N2 | 0.8743 (3) | −0.0060 (2) | 0.8029 (2) | 0.0276 (4) | |
N3 | 0.7895 (3) | 0.4967 (2) | 0.2158 (2) | 0.0231 (4) | |
N4 | 0.7192 (3) | 0.2633 (2) | −0.0123 (2) | 0.0229 (4) | |
C1 | 0.6050 (3) | −0.1178 (3) | 0.7269 (2) | 0.0255 (5) | |
C2 | 0.8140 (3) | −0.1085 (3) | 0.7246 (2) | 0.0244 (5) | |
C3 | 0.8286 (3) | 0.3798 (3) | 0.1378 (2) | 0.0232 (5) | |
C4 | 0.6896 (3) | 0.3944 (3) | 0.0565 (2) | 0.0222 (4) | |
H9o | 0.239 (3) | 0.3481 (15) | 0.571 (2) | 0.021 (6)* | |
H1w1 | 0.038 (2) | 0.202 (3) | 0.652 (2) | 0.04 (1)* | |
H1w2 | 0.150 (4) | 0.110 (3) | 0.598 (2) | 0.03 (1)* | |
H1n1 | 0.522 (5) | 0.095 (3) | 0.731 (2) | 0.05 (1)* | |
H1n2 | 0.393 (2) | 0.010 (4) | 0.692 (3) | 0.06 (1)* | |
H1n3 | 0.553 (4) | 0.053 (3) | 0.629 (1) | 0.04 (1)* | |
H2n1 | 0.841 (4) | 0.087 (2) | 0.792 (2) | 0.03 (1)* | |
H2n2 | 0.993 (2) | −0.010 (4) | 0.808 (2) | 0.04 (1)* | |
H2n3 | 0.818 (4) | −0.032 (3) | 0.860 (1) | 0.04 (1)* | |
H3n1 | 0.806 (4) | 0.585 (2) | 0.189 (2) | 0.04 (1)* | |
H3n2 | 0.874 (3) | 0.492 (3) | 0.258 (2) | 0.04 (1)* | |
H3n3 | 0.685 (3) | 0.502 (4) | 0.251 (2) | 0.06 (1)* | |
H4n1 | 0.827 (2) | 0.267 (3) | −0.045 (2) | 0.04 (1)* | |
H4n2 | 0.634 (3) | 0.260 (4) | −0.054 (2) | 0.04 (1)* | |
H4n3 | 0.722 (4) | 0.177 (2) | 0.020 (2) | 0.04 (1)* | |
H1a | 0.587 (4) | −0.195 (3) | 0.679 (2) | 0.04 (1)* | |
H1b | 0.551 (3) | −0.141 (3) | 0.793 (1) | 0.03 (1)* | |
H2a | 0.877 (4) | −0.203 (2) | 0.737 (2) | 0.05 (1)* | |
H2b | 0.863 (3) | −0.074 (3) | 0.659 (1) | 0.03 (1)* | |
H3a | 0.820 (4) | 0.288 (2) | 0.176 (2) | 0.02 (1)* | |
H3b | 0.952 (2) | 0.399 (3) | 0.111 (2) | 0.05 (1)* | |
H4a | 0.566 (2) | 0.397 (3) | 0.087 (2) | 0.02 (1)* | |
H4b | 0.708 (4) | 0.484 (2) | 0.017 (2) | 0.04 (1)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0083 (2) | 0.0142 (2) | 0.0164 (2) | 0.0000 (1) | −0.0007 (1) | −0.0004 (2) |
Fe2 | 0.0085 (2) | 0.0142 (2) | 0.0136 (2) | −0.0012 (1) | −0.0016 (1) | 0.0002 (1) |
S1 | 0.0114 (2) | 0.0167 (2) | 0.0128 (2) | −0.0002 (2) | −0.0003 (2) | 0.0008 (2) |
S2 | 0.0118 (2) | 0.0127 (2) | 0.0151 (2) | −0.0009 (2) | −0.0012 (2) | −0.0007 (2) |
S3 | 0.0187 (3) | 0.0206 (3) | 0.0168 (3) | −0.0043 (2) | −0.0015 (2) | 0.0015 (2) |
O1 | 0.013 (1) | 0.029 (1) | 0.017 (1) | 0.001 (1) | −0.0017 (1) | 0.002 (1) |
O2 | 0.013 (1) | 0.024 (1) | 0.015 (1) | −0.005 (1) | 0.000 (1) | −0.001 (1) |
O3 | 0.025 (1) | 0.035 (1) | 0.016 (1) | −0.002 (1) | 0.001 (1) | −0.005 (1) |
O4 | 0.025 (1) | 0.017 (1) | 0.031 (1) | 0.000 (1) | 0.001 (1) | 0.004 (1) |
O5 | 0.013 (1) | 0.016 (1) | 0.031 (1) | 0.000 (1) | 0.001 (1) | −0.003 (1) |
O6 | 0.014 (1) | 0.016 (1) | 0.023 (1) | −0.002 (1) | −0.006 (1) | −0.001 (1) |
O7 | 0.023 (1) | 0.013 (1) | 0.028 (1) | −0.001 (1) | 0.000 (1) | 0.002 (1) |
O8 | 0.023 (1) | 0.035 (1) | 0.017 (1) | −0.005 (1) | −0.001 (1) | −0.003 (1) |
O9 | 0.010 (1) | 0.015 (1) | 0.020 (1) | −0.001 (1) | −0.002 (1) | 0.003 (1) |
O10 | 0.05 (1) | 0.061 (1) | 0.017 (1) | −0.018 (1) | −0.006 (1) | 0.006 (1) |
O11 | 0.023 (1) | 0.027 (1) | 0.048 (1) | 0.004 (1) | 0.004 (1) | 0.003 (1) |
O12 | 0.021 (1) | 0.035 (1) | 0.024 (1) | −0.011 (1) | 0.001 (1) | 0.002 (1) |
O13 | 0.030 (1) | 0.019 (1) | 0.041 (1) | −0.004 (1) | −0.011 (1) | −0.002 (1) |
O1w | 0.026 (1) | 0.022 (1) | 0.029 (1) | 0.004 (1) | −0.006 (1) | 0.000 (1) |
N1 | 0.017 (1) | 0.027 (1) | 0.027 (1) | −0.001 (1) | −0.004 (1) | −0.004 (1) |
N2 | 0.025 (1) | 0.028 (1) | 0.032 (1) | −0.008 (1) | −0.011 (1) | 0.006 (1) |
N3 | 0.025 (1) | 0.025 (1) | 0.020 (1) | −0.001 (1) | −0.005 (1) | 0.000 (1) |
N4 | 0.022 (1) | 0.027 (1) | 0.021 (1) | −0.001 (1) | −0.003 (1) | −0.003 (1) |
C1 | 0.022 (1) | 0.024 (1) | 0.032 (1) | −0.004 (1) | −0.008 (1) | 0.000 (1) |
C2 | 0.021 (1) | 0.026 (1) | 0.027 (1) | 0.003 (1) | −0.004 (1) | −0.002 (1) |
C3 | 0.023 (1) | 0.026 (1) | 0.021 (1) | 0.004 (1) | −0.003 (1) | −0.001 (1) |
C4 | 0.023 (1) | 0.024 (1) | 0.020 (1) | 0.003 (1) | −0.004 (1) | −0.001 (1) |
Geometric parameters (Å, º) top
Fe1—O1 | 2.094 (1) | N4—C4 | 1.483 (3) |
Fe1—O1i | 2.094 (1) | C1—C2 | 1.494 (3) |
Fe1—O5 | 1.983 (1) | C3—C4 | 1.513 (3) |
Fe1—O5i | 1.983 (1) | O9—H9o | 0.84 (1) |
Fe1—O9 | 1.951 (1) | O1w—H1w1 | 0.84 (1) |
Fe1—O9i | 1.951 (1) | O1w—H1w2 | 0.84 (1) |
Fe2—O2 | 2.044 (1) | N1—H1n1 | 0.85 (1) |
Fe2—O2ii | 2.044 (1) | N1—H1n2 | 0.85 (1) |
Fe2—O6 | 1.998 (1) | N1—H1n3 | 0.86 (1) |
Fe2—O6ii | 1.998 (1) | N2—H2n1 | 0.86 (1) |
Fe2—O9 | 1.962 (1) | N2—H2n2 | 0.85 (1) |
Fe2—O9ii | 1.962 (1) | N2—H2n3 | 0.85 (1) |
S1—O3 | 1.441 (2) | N3—H3n1 | 0.85 (1) |
S1—O4 | 1.458 (2) | N3—H3n2 | 0.85 (1) |
S1—O1 | 1.502 (1) | N3—H3n3 | 0.85 (1) |
S1—O2 | 1.509 (1) | N4—H4n1 | 0.86 (1) |
S2—O8 | 1.446 (2) | N4—H4n2 | 0.86 (1) |
S2—O7 | 1.459 (2) | N4—H4n3 | 0.86 (1) |
S2—O6 | 1.493 (1) | C1—H1a | 0.95 (1) |
S2—O5 | 1.496 (2) | C1—H1b | 0.95 (1) |
S3—O10 | 1.461 (2) | C2—H2a | 0.95 (1) |
S3—O11 | 1.475 (2) | C2—H2b | 0.95 (1) |
S3—O12 | 1.475 (2) | C3—H3a | 0.94 (1) |
S3—O13 | 1.477 (2) | C3—H3b | 0.94 (1) |
N1—C1 | 1.486 (3) | C4—H4a | 0.94 (1) |
N2—C2 | 1.482 (3) | C4—H4b | 0.94 (1) |
N3—C3 | 1.477 (3) | | |
| | | |
O1—Fe1—O1i | 180 | N4—C4—C3 | 108.9 (2) |
O1—Fe1—O5 | 87.99 (6) | H1w1—O1w—H1w2 | 102 (3) |
O1—Fe1—O5i | 92.01 (6) | C1—N1—H1n1 | 110 (2) |
O1—Fe1—O9 | 91.53 (6) | C1—N1—H1n2 | 108 (2) |
O1—Fe1—O9i | 88.47 (6) | H1n1—N1—H1n2 | 104 (3) |
O5—Fe1—O5i | 180 | C1—N1—H1n3 | 114 (2) |
O5—Fe1—O9 | 91.13 (6) | H1n1—N1—H1n3 | 110 (3) |
O5—Fe1—O9i | 88.87 (6) | H1n2—N1—H1n3 | 111 (3) |
O9i—Fe1—O9 | 180 | C2—N2—H2n1 | 113 (2) |
O2—Fe2—O2ii | 180 | C2—N2—H2n2 | 113 (2) |
O2—Fe2—O6 | 90.99 (6) | H2n1—N2—H2n2 | 108 (3) |
O2—Fe2—O6ii | 89.00 (6) | C2—N2—H2n3 | 108 (2) |
O2—Fe2—O9 | 91.61 (6) | H2n1—N2—H2n3 | 106 (3) |
O2—Fe2—O9ii | 88.39 (6) | H2n2—N2—H2n3 | 110 (3) |
O6—Fe2—O6ii | 180 | C3—N3—H3n1 | 109 (2) |
O6—Fe2—O9 | 88.39 (6) | C3—N3—H3n2 | 110 (2) |
O6—Fe2—O9ii | 91.61 (6) | H3n1—N3—H3n2 | 102 (3) |
O9—Fe2—O9ii | 180 | C3—N3—H3n3 | 121 (2) |
O3—S1—O4 | 112.8 (1) | H3n1—N3—H3n3 | 106 (3) |
O3—S1—O1 | 109.3 (1) | H3n2—N3—H3n3 | 106 (3) |
O4—S1—O1 | 110.2 (1) | C4—N4—H4n1 | 110 (2) |
O3—S1—O2 | 108.5 (1) | C4—N4—H4n2 | 112 (2) |
O4—S1—O2 | 108.3 (1) | H4n1—N4—H4n2 | 110 (3) |
O1—S1—O2 | 107.7 (1) | C4—N4—H4n3 | 113 (2) |
O8—S2—O7 | 112.1 (1) | H4n1—N4—H4n3 | 104 (3) |
O8—S2—O6 | 110.2 (1) | H4n2—N4—H4n3 | 107 (3) |
O7—S2—O6 | 108.7 (1) | N1—C1—H1a | 107 (2) |
O8—S2—O5 | 109.7 (1) | C2—C1—H1a | 103 (2) |
O7—S2—O5 | 107.0 (1) | N1—C1—H1b | 108 (2) |
O6—S2—O5 | 108.9 (1) | C2—C1—H1b | 112 (2) |
O10—S3—O11 | 111.3 (1) | H1a—C1—H1b | 113 (2) |
O10—S3—O12 | 109.1 (1) | N2—C2—H2a | 105 (2) |
O11—S3—O12 | 107.9 (1) | C1—C2—H2a | 114 (2) |
O10—S3—O13 | 110.1 (1) | N2—C2—H2b | 109 (2) |
O11—S3—O13 | 108.7 (1) | C1—C2—H2b | 110 (2) |
O12—S3—O13 | 109.7 (1) | H2a—C2—H2b | 106 (2) |
S1—O1—Fe1 | 136.20 (9) | N3—C3—H3a | 103 (2) |
S1—O2—Fe2 | 132.86 (8) | C4—C3—H3a | 113 (2) |
S2—O5—Fe1 | 134.20 (9) | N3—C3—H3b | 104 (2) |
S2—O6—Fe2 | 137.17 (9) | C4—C3—H3b | 112 (2) |
Fe1—O9—Fe2 | 131.52 (7) | H3a—C3—H3b | 113 (2) |
Fe1—O9—H9o | 117 (2) | N4—C4—H4a | 111 (2) |
Fe2—O9—H9o | 109 (2) | C3—C4—H4a | 110 (2) |
N1—C1—C2 | 113.3 (2) | N4—C4—H4b | 107 (2) |
N2—C2—C1 | 112.3 (2) | C3—C4—H4b | 111 (2) |
N3—C3—C4 | 111.1 (2) | H4a—C4—H4b | 109 (2) |
| | | |
O3—S1—O1—Fe1 | −158.8 (1) | O1—Fe1—O5—S2 | 95.0 (1) |
O4—S1—O1—Fe1 | 76.8 (2) | O1i—Fe1—O5—S2 | −85.0 (1) |
O2—S1—O1—Fe1 | −41.1 (2) | O8—S2—O6—Fe2 | −75.2 (2) |
O9i—Fe1—O1—S1 | −144.2 (1) | O7—S2—O6—Fe2 | 161.5 (1) |
O9—Fe1—O1—S1 | 35.8 (1) | O5—S2—O6—Fe2 | 45.3 (2) |
O5i—Fe1—O1—S1 | 124.7 (1) | O9—Fe2—O6—S2 | −8.9 (1) |
O5—Fe1—O1—S1 | −55.3 (1) | O9ii—Fe2—O6—S2 | 171.1 (1) |
O3—S1—O2—Fe2 | 168.0 (1) | O2ii—Fe2—O6—S2 | 79.5 (1) |
O4—S1—O2—Fe2 | −69.4 (1) | O2—Fe2—O6—S2 | −100.5 (1) |
O1—S1—O2—Fe2 | 49.8 (1) | O5i—Fe1—O9—Fe2 | −132.2 (1) |
O9—Fe2—O2—S1 | −49.7 (1) | O5—Fe1—O9—Fe2 | 47.8 (1) |
O9ii—Fe2—O2—S1 | 130.3 (1) | O1—Fe1—O9—Fe2 | −40.2 (1) |
O6ii—Fe2—O2—S1 | −141.3 (1) | O1i—Fe1—O9—Fe2 | 139.8 (1) |
O6—Fe2—O2—S1 | 38.7 (1) | O6ii—Fe2—O9—Fe1 | 134.3 (1) |
O8—S2—O5—Fe1 | 80.2 (1) | O6—Fe2—O9—Fe1 | −45.7 (1) |
O7—S2—O5—Fe1 | −157.9 (1) | O2ii—Fe2—O9—Fe1 | −134.7 (1) |
O6—S2—O5—Fe1 | −40.5 (2) | O2—Fe2—O9—Fe1 | 45.3 (1) |
O9i—Fe1—O5—S2 | −176.5 (1) | N1—C1—C2—N2 | 71.2 (3) |
O9—Fe1—O5—S2 | 3.5 (1) | N3—C3—C4—N4 | −172.8 (2) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O9—H9o···O1w | 0.84 (1) | 1.94 (1) | 2.757 (2) | 164 (2) |
O1w—H1w1···O4ii | 0.84 (1) | 2.18 (1) | 2.988 (2) | 163 (3) |
O1w—H1w2···O7iii | 0.84 (1) | 1.99 (1) | 2.790 (2) | 159 (3) |
N1—H1n1···O12i | 0.85 (1) | 2.14 (2) | 2.912 (3) | 151 (3) |
N1—H1n2···O8iii | 0.85 (1) | 2.32 (3) | 2.966 (3) | 132 (3) |
N1—H1n3···O7i | 0.86 (1) | 2.17 (2) | 2.967 (3) | 153 (3) |
N1—H1n2···O1w | 0.85 (1) | 2.30 (3) | 2.923 (3) | 130 (3) |
N2—H2n1···O4i | 0.86 (1) | 2.04 (1) | 2.847 (3) | 158 (3) |
N2—H2n2···O13iv | 0.85 (1) | 2.05 (2) | 2.840 (3) | 155 (3) |
N2—H2n3···O10v | 0.85 (1) | 1.88 (1) | 2.714 (3) | 165 (3) |
N3—H3n1···O11 | 0.85 (1) | 2.02 (1) | 2.842 (3) | 161 (3) |
N3—H3n2···O2vi | 0.85 (1) | 2.07 (1) | 2.912 (2) | 174 (3) |
N3—H3n3···O1 | 0.85 (1) | 2.12 (1) | 2.964 (2) | 176 (3) |
N4—H4n1···O11vii | 0.86 (1) | 1.97 (1) | 2.811 (3) | 168 (3) |
N4—H4n2···O12viii | 0.86 (1) | 1.96 (1) | 2.807 (3) | 169 (3) |
N4—H4n3···O13iii | 0.86 (1) | 1.99 (1) | 2.834 (3) | 165 (3) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+1, −z+1; (iii) x, y−1, z; (iv) −x+2, −y+1, −z+1; (v) x, y−1, z+1; (vi) x+1, y, z; (vii) −x+2, −y+1, −z; (viii) −x+1, −y+1, −z. |