Crystallography relevant to Mars and Galilean icy moons: crystal behavior of kieserite-type monohydrate sulfates at extraterrestrial conditions down to 15 K

Wildner, M.; Zakharov, B.A.; Bogdanov, N.E.; Talla, D.; Boldyreva, E.V.; Miletich, R.

doi:10.1107/S2052252521012720

research papers

IUCrJ

Volume 9| Part 2| March 2022| Pages 194-203

ISSN: 2052-2525

https://doi.org/10.1107/S2052252521012720

CHEMISTRY | CRYSTENG

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Crystallography relevant to Mars and Galilean icy moons: crystal behavior of kieserite-type monohydrate sulfates at extraterrestrial conditions down to 15 K

Manfred Wildner,^a ^* Boris A. Zakharov,^b,^c Nikita E. Bogdanov,^b,^c Dominik Talla,^a Elena V. Boldyreva ^b,^c and Ronald Miletich ^a

^aDepartment of Mineralogy and Crystallography, University of Vienna, Althanstraße 14, A-1090 Wien, Austria, ^bBoreskov Institute of Catalysis, Siberian Branch of the Russian Academy of Sciences, Lavrentieva Avenue 5, Novosibirsk 630090, Russian Federation, and ^cNovosibirsk State University, Pirogova Street 2, Novosibirsk 630090, Russian Federation
^*Correspondence e-mail: manfred.wildner@univie.ac.at

Edited by P. Lightfoot, University of St Andrews, United Kingdom (Received 13 October 2021; accepted 30 November 2021; online 11 January 2022)

Monohydrate sulfate kieserites (M²⁺SO₄·H₂O) and their solid solutions are essential constituents on the surface of Mars and most likely also on Galilean icy moons in our solar system. Phase stabilities of end-member representatives (M²⁺ = Mg, Fe, Co, Ni) have been examined crystallographically using single-crystal X-ray diffraction at 1 bar and temperatures down to 15 K, by means of applying open He cryojet techniques at in-house laboratory instrumentation. All four representative phases show a comparable, highly anisotropic thermal expansion behavior with a remarkable negative thermal expansion along the monoclinic b axis and a pronounced anisotropic expansion perpendicular to it. The lattice changes down to 15 K correspond to an `inverse thermal pressure' of approximately 0.7 GPa, which is far below the critical pressures of transition under hydrostatic compression (P_c ≥ 2.40 GPa). Consequently, no equivalent structural phase transition was observed for any compound, and neither dehydration nor rearrangements of the hydrogen bonding schemes have been observed. The M²⁺SO₄·H₂O (M²⁺ = Mg, Fe, Co, Ni) end-member phases preserve the kieserite-type C2/c symmetry; hydrogen bonds and other structural details were found to vary smoothly down to the lowest experimental temperature. These findings serve as an important basis for the assignment of sulfate-related signals in remote-sensing data obtained from orbiters at celestial bodies, as well as for thermodynamic considerations and modeling of properties of kieserite-type sulfate monohydrates relevant to extraterrestrial sulfate associations at very low temperatures.

Keywords: monohydrate sulfate kieserites; Galilean icy moons; He cryojet techniques.

CCDC references: 2067136; 2067139; 2067140; 2125292; 2125293; 2125294; 2125295; 2125296; 2125297; 2125298; 2125299; 2125300; 2125301; 2125302; 2125303; 2125304; 2125305; 2125306; 2125307; 2125308; 2125309; 2125310; 2125311; 2125312; 2125313; 2125314; 2125315; 2125316; 2125317; 2125318; 2125319; 2125320; 2125321; 2125322

1. Introduction

The abundance of sulfate minerals, in particular hydrated magnesium sulfates (MgSO₄·nH₂O), has been confirmed on Mars and elsewhere in the solar system starting with the first in situ discovery in martian soils by the Viking Mars probe (Keil et al., 1978 ; Clark & Van Hart, 1981 ). The ability of these materials to release or absorb water and the prevailing humidity, even forming liquid brines (Peterson & Wang, 2006 ), ranks them among critical components governing the water cycles on the surface of Mars and other celestial bodies. The influence of temperature, humidity and pressure on dehydration and rehydration capabilities has been investigated in various laboratory studies (e.g. Wang et al., 2009 ; Nakamura & Ohtani, 2011 ; Fortes et al., 2017a ). Among these MgSO₄·nH₂O phases, covering a wide range of hydration states (n) from 0 to 11, the monohydrate sulfate kieserite and its solid solutions with transition metal (TM) counterparts (Papike et al., 2007 ) dominate the deposits at lower martian latitudes, where it is assumed to be an essential H₂O carrier (e.g. Christensen et al., 2004 ; Arvidson et al., 2005 ; Clark et al., 2005 ; Bishop et al., 2009 ).

However, there is some ongoing dispute regarding the stability of kieserite on the martian surface. On the one hand, Chipera & Vaniman (2007 ) argue that the relative humidity should lead to its rehydration to starkeyite, MgSO₄·4H₂O, which is thermodynamically stable under the prevailing conditions. On the other hand, Wang et al. (2009) found that the presence of Ca- and Fe-sulfates and Fe-oxides or Fe-hydroxides enhances the dehydration of higher Mg-sulfates down to the monohydrate. Smectite minerals were shown to have a stabilizing effect on the hydration states, allowing lower sulfate hydrates to exist well outside their stability range (Wilson & Bish, 2012 ). Furthermore, there is evidence that martian kieserite actually has an intermediate composition between the end members kieserite, MgSO₄·H₂O, and szomolnokite, FeSO₄·H₂O (Bishop et al., 2009). The respective synthetic materials used for the investigation of the given solid solution (Talla & Wildner, 2019 ) show no sign of rehydration even after several years under ambient conditions as soon as the Fe content exceeds 0.2 apfu.

A related debate concerns the existence and nature of a postulated second structural polytype of kieserite with a broader stability range but similar spectroscopic properties, the so-called low-humidity (LH) kieserite, presumed by several authors to prevail on Mars (Wang et al., 2009; Jamieson et al., 2014 ). While elucidation of the actual structure and properties of this enigmatic `LH phase' is still pending to date, it is one of the goals of the present study to provide reliable – hitherto missing – low-temperature reference data of `classical' MSO₄·H₂O compounds, to serve as a benchmark for comparison and as a basis for spectroscopic and thermodynamic modeling purposes.

Spectroscopic data recorded by orbiters reveal sulfate-rich regions to be present not only on the martian surface, but also appear to be an abundant feature on many other celestial bodies in our solar system, i.e. on the icy moons of Jupiter and Saturn (Kargel, 1991 ; McCord et al., 2001a ). Higher hydrated Mg-sulfates (n = 6–11) are assumed to be relevant non-ice mineral constituents on the surface but also in the ice mantles of the Galilean moons (e.g. McCord et al., 2001a; Dalton et al., 2005 , 2012 ). While McCord et al. (2001b ) did not find any indication of Mg-sulfate radiolysis when subjecting epsomite (n = 7) to a 100 eV electron beam, Tani et al. (2012 ) determined the formation of hydrogen and sulfite radicals at 90 K by exposure to gamma radiation. More importantly, several studies have shown that the interaction of UV or other energetic radiation with highly hydrated sulfates significantly catalyzes and speeds up their dehydration. Under such influence, epsomite is converted to hexahydrite [the mineral name for the hexahydrate, MgSO₄·6H₂O (Cardell et al., 2007 )], the further dehydration of which has also been proven to be catalyzed by UV radiation (Cloutis et al., 2007 ). This processes could lead to the formation of sulfate monohydrates on the icy surface of the Galilean moons.

Moreover, lower-hydrated or even anhydrous sulfates are also expected to be present within the deeper mantle and core of these planetary bodies (Kargel, 1991; Nakamura & Ohtani, 2011; Meusburger et al., 2020 ). Depending on their thermodynamic stability, they play a key role for the formation of subsurface oceans, which could even contain extraterrestrial life, as discussed for the south-polar region of Saturn's moon Enceladus, where a subsurface body of liquid exists due to tidal heating (Solomonidou et al., 2011 ). However, no clear confirmation of the presence of sulfates on this latter object or in its hydrothermal plumes exists, in part because of significant overlaps of rather broad bands and combination modes of various sulfate minerals in the standard <5 µm spectral range covered by orbiters (Bishop et al., 2004 ). This problem becomes even more remarkable when the deposits are spatially restricted with other phases present, necessitating the use of complex spectral unmixing models (e.g. Combe et al., 2008 ). However, it is most probable that the rocky core of the moon corresponds to C1/C2 chondritic composition (Kargel, 1991; Sekine et al., 2015 ), where high sulfate contents are present in the soluble fraction (Fredriksson & Kerridge, 1988 ; Burgess et al., 1991 ), filling abundant brecciation cracks (Richardson, 1978 ); therefore the presence of sulfates also on Enceladus will probably be confirmed by future missions.

Following our investigations on the structural crystallography of kieserite-type solid solutions: M²⁺SO₄·H₂O (M²⁺ = Mg, Fe, Co, Ni), including the temperature-dependent behavior of the end members at temperatures prevailing at equatorial martian latitudes (Bechtold & Wildner, 2016 ; Talla & Wildner, 2019; Talla et al., 2020 ), we recently carried out investigations under high-pressure conditions relevant to the interior of individual icy moons (Meusburger et al., 2019 , 2020; Ende et al., 2020 ; Wildner et al., 2021 ). These experimental studies revealed a second-order phase transition from the monoclinic α-phase (space group C2/c) to a triclinic β-phase (space group P1) at critical transition pressures ranging from 2.40 (Co) to 6.15 GPa (Fe). The findings from high-pressure crystallography show a partial rearrangement of the hydrogen-bonding scheme as the most obvious structural change. Earlier studies down to 110 K (Talla & Wildner, 2019, Talla et al., 2020) gave no evidence of a comparable transition, however, it can not be ruled out to occur at temperatures even lower than the previously covered range. Although on Mars the temperatures in equatorial latitudes range between 280 and 170 K (Witzke et al., 2007 ), significantly lower temperatures can be expected on the surface of the icy satellites. The temperature changes during the seasonal and diurnal cycles on some of the icy moons of Jupiter and Saturn have been modeled, such as for Europa (Ashkenazy, 2019 ), where the mean annual temperature range spans (depending on the assumed internal heating rate) from 94 to 98 K in equatorial latitudes and from 35 to 62 K on the poles. The measurements during the Rosetta mission to comet 67P showed evidence of SO₂ in its plume and ammonium sulfate on its surface, suggesting the presence of sulfate on cometary bodies and asteroids (Poch et al., 2020 ). In such cases, they are exposed to temperatures as low as those of the cosmic vacuum, amounting to a mere 2.7 K.

Since the reliable knowledge of phase relations and structural details of relevant sulfate minerals at astrophysically significant conditions is of utmost importance for their identification and discrimination in remote-sensing spectroscopic data from orbiters, we extend our investigations on end-member monohydrate sulfates well down to temperatures as low as 15 K. To reveal the structural changes, in situ low-temperature X-ray crystallography was carried out at temperature conditions relevant to the icy moons of Jupiter and Saturn and comparable objects in the outer solar system, as well as the polar regions of Mars or dwarf planets and asteroids within the inner solar system. At the same time, this study aims to verify any potential structural phase transition equivalent to those reported earlier under compression of kieserite-type phases, following the analogy of `inverse thermal pressure' on cooling.

2. Experimental

2.1. Temperature-dependent single-crystal X-ray data collection

Single crystals of synthetic kieserite-type compounds M²⁺SO₄·H₂O (M²⁺ = Mg, Fe, Co, Ni) for the present data collections were extracted from the respective end-member batches prepared earlier (Bechtold & Wildner, 2016; Talla & Wildner, 2019; Talla et al., 2020). Data collections between 313 and 113 K were performed in steps of 40 K on a Bruker Apex II diffractometer equipped with a CCD area detector and an Incoatec Microfocus Source IµS (30 W, multilayer mirror, Mo Kα), in a dry stream of nitrogen (Cryostream 800, Oxford Cryosystems). Several sets of φ- and ω-scans with a 2° scan width were measured at a crystal–detector distance of 40 mm up to 80° 2θ full sphere. Absorption was corrected by evaluation of multi-scans. Measurements and correction procedures were performed with the SAINT software package (Bruker AXS, 2012 ). Data collections between 75 and 15 K (and at room temperature) were performed in steps of 15 K with Mo Kα radiation on an Oxford Diffraction Gemini R Ultra diffractometer with a CCD detector. The open-flow helium cryostat Helijet from Oxford Diffraction with helium coaxial flow shielding was used to maintain low temperatures of the samples. Data collections and treatments were performed using CrysAlisPro software (Rigaku Oxford Diffraction, 2016 $[Rigaku Oxford Diffraction (2016). CrysAlis PRO. Rigaku Oxford Diffraction, The Woodlands, Texas, USA.]$ ). During several of the scheduled measurements we encountered a problem of excessive formation of an 'ice'-cover on the sample crystals, composed from solidified air components, mainly O₂ and N₂, in the open-flow helium cryostat, leading to interference of sample reflections with the emergent multi-grain powder rings (see Zakharov et al., 2021 ). These datasets were excluded from consideration: respective data collections were aborted and/or deleted from the further analyses. Data collection was resumed after the problem was fixed or, at least, partly solved by changing the crystal holder type and other preventive measures.

2.2. Crystal structure refinements

All structure refinements were performed on F² with SHELXL (Sheldrick, 2015 ) in the `traditional' non-reduced kieserite cell setting (cf. Wildner & Giester, 1991 ) in the space group C2/c. Scattering curves for neutral atoms were used. Note that, for the purposes of data consistency and comparability, the cell axis parameters from the temperature-dependent measurements were corrected in such a way that respective values at 293 K (interpolated for Apex II measurements) match those from earlier room-temperature (RT) studies, obtained on a Nonius Kappa CCD diffractometer (see Bechtold & Wildner, 2016; Talla & Wildner, 2019; Talla et al., 2020), since the latter RT data proved to most closely match corresponding high-precision lattice parameters obtained with the 8-position centering mode (King & Finger, 1979 ) on a Stoe AED II diffractometer. The respective corrections were in the range ≤2‰. Further note that the structures of the Mg and Fe compounds at 193 and 113 K have already been published by Talla & Wildner (2019) and those of NiSO₄·H₂O at 273, 193 and 113 K by Talla et al. (2020). Crystal structure drawings throughout the paper were prepared with the program VESTA3 (Momma & Izumi, 2011 ).

2.3. Thermal equation of state calculations

Due to the limited number of temperature-dependent unit-cell data points (8–10 at most) obtained from full single-crystal structure determinations, we preferred to keep the thermal equation of state (EoS) analyses as simple as possible and with a minimum of variable parameters. The unit-cell axes lengths and cell volumes between 15 and 313 K were fitted therefore to a Fei-type (Fei, 1995 ) thermal EoS using the EoSFit7c and EoSFit7-GUI programs by Angel and coworkers (Angel et al., 2014 ; Gonzalez-Platas et al., 2016 ). The reference temperature was chosen at T_ref = 293 K; α₂ was fixed at 0 (see also Angel et al., 2014), i.e. simplifying the thermal EoS to the linear approach with two coefficients following α = α₀ + α₁T. Strain and thermal expansion tensors were calculated from the thermal EoS with the Strain utility in the EoSFit7c program.

3. Results and discussion

3.1. General aspects

Selected crystal data and details of the data collections and structure refinements are summarized in Table S1 of the supporting information. Final atomic parameters are listed in Table S2, and results of the thermal EoS and strain calculations in Table 1. The most relevant interatomic distances and angles are given in Table S3. Under ambient conditions, kieserite and isotypic compounds M²⁺SO₄·H₂O (M²⁺ = Mg, Fe, Co, Ni) crystallize with monoclinic symmetry in the space group C2/c (Hawthorne et al., 1987 ; Wildner & Giester, 1991). The crystal structure of the Mg-representative kieserite is illustrated in Fig. 1 projected along the crystallographic c axis. The structures are built from kinked chains of O3(H₂O)-corner-sharing MO₄(H₂O)₂ octahedra (point symmetry 1), elongated along their O3–O3 axes, and nearly regular SO₄ tetrahedra (point symmetry 2), intra-linking adjacent octahedra within the chains by common O2 corners. These octahedral–tetrahedral chains are aligned parallel to the c axis (i.e. along the viewing direction in Fig. 1) and interlinked to a framework by sharing the remaining polyhedral O1 corners as well as by moderately strong O3–H⋯O2 hydrogen bonds.

Table 1
Results of Fei-type thermal EoS and strain tensor calculations for kieserite-type compounds M²⁺SO₄·H₂O (M²⁺ = Mg, Fe, Co, Ni) for T_ref = 293 K using EoSFit7c (Angel et al., 2014)

Values of α are given as α × 10⁻⁵ K⁻¹, α₀ × 10⁵ K⁻¹ and α₁ × 10⁸ K⁻². The parameter α₂ was fixed at α₂ = 0. Strain tensor components e_ij (based on Cartesian axes X // a*, Y // b, Z // c) are given for 113 K.

	Mg	Fe	Co	Ni
α_V,293	3.41 (65)	4.66 (49)	3.34 (28)	3.55 (37)
V₀	355.75 (5)	365.65 (6)	354.77 (3)	342.98 (3)
α_0(V)	0.5 (7)	0.3 (5)	1.4 (3)	−1.7 (4)
α_1(V)	10 (3)	15 (3)	6.7 (15)	18 (2)

α_a,293	5.89 (24)	4.49 (18)	4.28 (26)	2.76 (54)
a₀	6.9146 (4)	7.0863 (3)	6.9699 (3)	6.8289 (6)
α_0(a)	–0.4 (5)	1.58 (18)	1.2 (3)	0.7 (5)
α_1(a)	21.4 (12)	9.9 (9)	10.4 (13)	7(3)

α_b,293	–4.36 (30)	–1.71 (19)	–2.68 (16)	–0.79 (49)
b₀	7.6285 (6)	7.5545 (3)	7.5947 (3)	7.6048 (7)
α_0(b)	0.6 (3)	–0.98 (19)	–0.34 (16)	–1.4 (5)
α_1(b)	–17.0 (15)	–2.5 (10)	–8.0 (8)	2(3)

α_c,293	4.05 (21)	3.31 (16)	2.95 (24)	3.04 (40)
c₀	7.6429 (4)	7.7802 (3)	7.6321 (4)	7.4625 (5)
α_0(c)	–0.3 (2)	0.76 (16)	1.8 (2)	–1.3 (4)
α_1(c)	14.8 (10)	8.7 (8)	4.0 (12)	15 (2)

e₁₁	–0.00468 (6)	–0.00416 (6)	–0.00390 (7)	–0.00216 (14)
e₂₂	0.00522 (6)	0.00279 (6)	0.00339 (7)	0.00172 (13)
e₃₃	–0.00491 (6)	–0.00452 (7)	–0.00446 (8)	–0.00342 (14)
e₁₃	0.00300 (3)	0.00266 (3)	0.00214 (3)	0.00155 (6)

Figure 1
Crystal structure of kieserite (MgSO₄·H₂O) at 15 K, projected along the c axis, i.e. along the octahedral–tetrahedral chains.

3.2. Thermal expansion of the unit cell

The lattice dimensions, depicted in Fig. 2, as well as the structural properties of the kieserite-group representatives deviate more or less from a linear fashion with decreasing temperature. While approximately linear shifts of lattice parameters are usually observed in high-temperature studies from RT upwards, the tendency to flatten below around 100 K towards absolute zero is well known for many crystalline solids (e.g. Drebushchak, 2020 ), and even an inversion of the trends leading to negative bulk volume expansion may be observed below ∼50 K; respective examples among sulfates are higher hydrates like meridianiite [MgSO₄·11H₂O (Fortes et al., 2008 )] or mirabilite [Na₂SO₄·10H₂O (Brand et al., 2009 )].

Figure 2
Unit-cell dimensions of kieserite-type compounds M²⁺SO₄·H₂O (M²⁺ = Mg, Fe, Co, Ni) in the temperature range 15–313 K with lines representing the Fei-type EoS results (Table 1

): (a) a and c axes; (b) b axes; (c) unit-cell volumes; and (d) monoclinic angle β. For errors see the underlying data in Tables 1

, S1 and S2.

The thermal expansion parameters and Fei-type EoS coefficients of the title compounds are summarized in Table 1. As expected, the cell volumes decrease on cooling [Fig. 2(c)], as do the a and c axes and the monoclinic angle β [Figs. 2(a) and 2(d)], whereas the b axes lengthen in all four compounds over the full investigated temperature range [Fig. 2(b)], showing a pronounced negative thermal expansion (NTE) effect. The present NTE behavior is even more remarkable since, with α_b,293 ranging between −4.4 × 10⁻⁵ K⁻¹ in kieserite (Mg) and −0.8 × 10⁻⁵ K⁻¹ in NiSO₄·H₂O, it amounts to a magnitude comparable to the positive thermal expansion of the a and c axes, and it furthermore shows no sign of turning positive or at least flattenning towards higher temperatures. NTE behavior of single lattice axes in otherwise `thermally normal' compounds is not uncommon, but usually at a much lower rate. For example, in epsomite (MgSO₄·7H₂O) and meridianiite (MgSO₄·11H₂O) each one of their lattice axes shows NTE (in the former case with an already high α of at most −2 × 10⁻⁵ K⁻¹), both turning positive at ∼250 K (Fortes et al., 2006 , 2008); in chalcanthite, CuSO₄·5H₂O, a very weak axial NTE is observed which flattens towards ∼300 K (Schofield & Knight, 2000 ). The strong NTE effect of the b axes in the title compounds is further discussed below (Section 3.4).

Regarding the bulk volume thermal expansion α_V [Table 1, Fig. 2(c)], the Fe compound with the largest cell volume also shows the strongest volume expansion (4.7 × 10⁻⁵ K⁻¹), while, within limits of error, the Mg and Co compounds (similar cell volumes) but also the Ni phase with the smallest cell volume, all have the same smaller volume expansion (∼3.4 × 10⁻⁵ K⁻¹). The flattening of the cell volumes towards low temperatures seems to be somewhat more pronounced in the Ni and Mg phases compared with those of Co and especially Fe. MgSO₄·H₂O consistently exhibits the strongest changes of the individual cell-edge lengths with temperature, especially concerning the excessive negative thermal expansion of the b axes, whereas NiSO₄·H₂O shows a significantly smaller average change of the axial lengths [Figs. 2(a) and 2(b)]. Among the four compounds, the a axes show a slightly higher expansion than the c axes, apart from the insignificant inversion in NiSO₄·H₂O (Table 1).

The respective thermal expansion tensors depicted in Figs. 3(a) and 3(b) (derived from the strain components in Table 1) exhibit pronounced anisotropy also in the plane perpendicular to the NTE-affected b axes, not evident from the more or less similar thermal expansion values α_a,c of the a and c axes (Table 1). As illustrated in Fig. 3(b), the respective smallest positive eigenvalues are oriented approximately parallel to the short cell diagonal in the ac plane, the largest ones approximately parallel to [201]. For the Ni compound, these directions deviate slightly (∼9°) from the quite consistent orientation in the other compounds. The relation between the anisotropy of thermal expansion and stereochemical changes with temperature is further discussed in Section 3.4.

Figure 3
(a) Thermal expansion tensor in MgSO₄·H₂O at 113 K (T_ref = 293 K), with green indicating positive values, red indicating negative values; (b) cross sections of the thermal expansion tensors of kieserite-type compounds M²⁺SO₄·H₂O (M²⁺ = Mg, Fe, Co, Ni) at 113 K (T_ref = 293 K) in the ac plane, superimposed on a respective projection of the structure of kieserite at 113 K. For increasing temperature, black arrows show the sense of tetrahedral rotations around the twofold axis, red arrows indicate the resulting opposing translations of neighboring octahedral–tetrahedral chains within the ac plane (see text). The tensor surface and cross sections were prepared with the program WinTensor (Kaminski, 2014

The volume thermal expansion α_V of the investigated kieserite-type compounds compares well with that of anhydrous sulfates. For example, in α- and β-MgSO₄ the values at 300 K are 3.7 × 10⁻⁵ and 4.1 × 10⁻⁵ K⁻¹, respectively (Fortes et al., 2007 ), in anhydrite (CaSO₄) it is 3.7 × 10⁻⁵ K⁻¹ at RT (Evans, 1979 ). Higher hydrated sulfates usually also exhibit larger thermal expansion coefficients at or close to RT: in gypsum [CaSO₄·2H₂O (Schofield et al., 1996 )] α_V is 7.0 × 10⁻⁵ K⁻¹ (320 K), in epsomite [MgSO₄·7H₂O (Fortes et al., 2006)] it is 11 × 10⁻⁵ K⁻¹ (300 K), in MgSO₄·9H₂O (Fortes et al., 2017b ) it is 11.3 × 10⁻⁵ K⁻¹ (250 K), in mirabilite [Na₂SO₄·10H₂O (Brand et al., 2009)] it is 11 × 10⁻⁵ K⁻¹ (300 K) and in meridianiite [MgSO₄·11H₂O (Fortes et al., 2008] it is 7.2 × 10⁻⁵ K⁻¹ (250 K).

As a major result of the present investigation, we observed no evidence suggesting a structural phase transition in any of the four investigated compounds within the studied temperature range, i.e. all four title compounds keep the monoclinic C2/c symmetry that the kieserite structure type features under ambient conditions. Note that a magnetic order–disorder transition was reported for FeSO₄·H₂O at 29.6 K using Mössbauer spectroscopy (Van Alboom et al., 2009 ), which is, however, not expected to be detectable in X-ray diffraction studies. Bearing in mind that high-pressure phase transitions in the investigated compounds occur at critical pressures P_c ≥ 2.40 GPa (Meusburger et al., 2019, 2020; Ende et al., 2020; Wildner et al., 2021), corresponding to cell volume ratios V/V₀ ≤ 0.96, whereas the intrinsic `thermal pressure' (e.g. Anderson, 1995 ) induced on cooling from RT to 15 K merely results in a volume decrease to roughly V/V₀ ≃ 0.993 (Fig. S1 of the supporting information), it becomes clear that phase transitions corresponding to those at high pressures were not to be expected. This also means that kieserite-type compounds and very probably also their solid solutions will not undergo structural transitions at or close to the surface of sulfate-bearing celestial bodies. The relationships of changes in cell and crystal chemical parameters on cooling versus pressure increase are further discussed in detail in the respective sections below.

3.3. Unit-cell thermal expansion versus compressibility

Compared with the temperature-dependent changes in lattice dimensions discussed above, the high-pressure behavior of the title compounds, investigated recently by Meusburger et al. (2019, 2020), Ende et al. (2020) and Wildner et al. (2021) is characterized by a continuous second-order ferroelastic phase transition from the present monoclinic α-phase (C2/c) to a triclinic β-phase (space group P1) at pressures of 2.72, 6.15, 2.40 and 2.47 GPa for M²⁺ = Mg, Fe, Co and Ni, respectively. Nevertheless, since the cells of the β-polymorphs are based on the respective reduced cells of the C2/c α-phase, a direct comparison of the lattice dimensions even across the phase transition is still feasible. However, such a comparison [see Tables S1, 1 and Figs. 2, S1 in the present work, and Table 2 in the work by Wildner et al. (2021)] shows that the ideally expected inverse relationship between compression and thermal expansion (e.g. Hazen & Finger, 1982a ) is approximately fulfilled for selected aspects only (Fig. S1).

On the one hand, the Fe compound revealing the highest volume thermal expansion α_V (Table 1) shows, as expected, the highest compressibility and thus the smallest bulk modulus of K₀ ≃ 45 GPa (Meusburger et al., 2019), albeit close to K₀ of the Mg and Co phases. The Ni compound with the clearly highest bulk modulus K₀ ≃ 60 GPa (Ende et al., 2020) also exhibits the smallest thermal changes of the axial lengths (〈α_|a,b,c|〉 ≃ 2.2 × 10⁻⁵ K⁻¹) but a volume thermal expansion comparable to the Mg and Co phases (Table 1). Among the individual cell axes, the softest c axis upon compression (〈M_c〉 ≃ 125 GPa) most closely follows the expectation of equal slopes in V/V₀ versus l/l₀ plots for pressure and temperature (〈α_c〉 ≃ 3.3 × 10⁻⁵ K⁻¹) in Fig. S1. On the other hand, in contrast to the expected inverse relationship, the clearly stiffest a axes upon compression (〈M_a〉 ≃ 395 GPa) exhibit the highest thermal expansion (〈α_a〉 ≃ 4.4·10⁻⁵ K⁻¹) and, finally, the NTE behavior (〈α_b〉 ≃ −2.4 × 10⁻⁵ K⁻¹) of the rather `soft' b axes (〈M_b〉 ≃ 145 GPa) is in harsh contradiction to all respective expectations.

The relationship referred to (Hazen & Finger, 1982a) is primarily expected for high-temperature structural studies, but the trends in Fig. 2 can evidently be extrapolated also to moderately higher temperatures, presumably up to the decomposition temperatures [≥300°C under dry conditions (Chipera et al., 2006 )]. Besides, the relationship is expected to fail for structures comprising polyhedra with grossly different ratios of expansivity versus compressibility (e.g. Sharp et al., 1987 ). While this is seemingly not the case in kieserite-type compounds with tetrahedral S—O bond lengths hardly responding to changes either in temperature (see below) or pressure (Wildner et al., 2021), the O—H⋯O hydrogen bonds in these compounds run within structural voids which in the topologically related structure of titanite, CaTiO(SiO₄), are occupied by the Ca atoms (Hawthorne et al., 1987). Hence, the hydrogen bonds in MSO₄·H₂O might play a major role for the clear deviation from respective expectations.

3.4. Polyhedral thermal expansion and crystal chemical changes

The octahedral volumes and mean M–O bond lengths decrease on cooling by reducing the two longest M–O3 bonds to the H₂O molecules [Fig. 4(a) and Table S3]. For the Fe compound, the bonds to O1 and O2 also seem to show a faint trend to lengthen and shorten, respectively, with reduced temperature; thus, for the FeO₆ octahedron the aberrant tendency towards a [2+2+2]-coordination (cf. Talla & Wildner, 2019; Wildner et al., 2021) still increases, compared with the clear and stable [4+2]-elongation of the other representatives. On average, the volumes of the MO₆ octahedra shrink with an α_V_oct of roughly 2.9 × 10⁻⁵ K⁻¹; in the Mg compound, for example, V_oct decreases by 0.7% from 11.90 to 11.82 Å³ from RT to 15 K, a rate comparable in magnitude to the MgO₆ octahedra in other magnesium sulfates, as listed by Fortes et al. (2008) – but excluding data from ultra-low T < 5 K. Along with the volume reduction, the octahedral bond length and angle distortions also decrease slightly with decreasing temperature for all four compounds.

Figure 4
Selected stereochemical parameters of kieserite-type compounds M²⁺SO₄·H₂O (M²⁺ = Mg, Fe, Co, Ni) in the temperature range 15–313 K with second-order regression lines. (a) Individual and mean M—O bond lengths, (b) O3—H⋯O2 hydrogen bond lengths, (c) M—O—S and M–O3–M angles at polyhedra-linking oxygen atoms, and (d) rotations of tetrahedral O1—O1′ and O2—O2′ edges relative to those in the Mg compound at 293 K. For errors see the underlying structural data in Tables S1, S2 and S3.

S—O bond lengths and the tetrahedral volume show an artificial increase on cooling owing to changes in thermal motion (Table S3), a phenomenon typically found for uncorrected bonds in small coordination polyhedra [e.g. data for sulfate groups listed by Fortes et al. (2008)]. In the present kieserite-type compounds, a `simple rigid bond' correction according to Downs et al. (1992 ) reveals almost constant 〈S—O〉 bond lengths over the full temperature range. Anyway, the observed difference of around 0.004 Å in the 〈S—O〉 distances in the Mg compound (shorter S—O bonds) compared with the TM representatives (longer S—O bonds) is maintained over the investigated temperature range. In the same range the O3—H⋯O2 hydrogen bond lengths reduce by roughly 0.03 Å, in case of the Ni phase by half that value [Fig. 4(b) and Table S3]. Somewhat surprisingly, the two O3—H⋯O1 contacts (around 3.3 Å under ambient conditions), which shorten under pressure (one of them forming a new hydrogen bond in the high-pressure β-MSO₄·H₂O polymorphs), significantly lengthen when the temperature is reduced. Since the O3—H⋯O1 contacts run nearly parallel to the b axis, this unexpected finding can be attributed to a side-effect of the axial NTE behavior. Polyhedra-linking angles [Fig. 4(c) and Table S3] also show a parallel response to temperature in all four compounds, despite the fact that both M–O–S angles (but especially M–O1–S) are substantially larger in MgSO₄·H₂O than in the TM phases, leading to, among other things, a volume mismatch of octahedral versus cell volume, especially eye-catching when comparing the Mg and Co compounds [as discussed in detail by Bechtold & Wildner (2016)]. While the octahedral chain angle M–O3–M remains almost constant on cooling to 15 K, the M–O–S angles become smaller by 0.4–1.1°. The resulting rotation of the SO₄ tetrahedron around its twofold symmetry axis [Figs. 4(d) and 5] has the same direction as that found for increasing pressure (Wildner et al., 2021) or increasing x_TM in (Mg,TM)SO₄·H₂O solid solutions (Bechtold & Wildner, 2016; Talla & Wildner, 2019; Talla et al., 2020). Within the studied temperature range, it amounts to roughly 1.1° for both O1—O1′ and O2—O2′ tetrahedral edges, but again clearly less in the Ni phase. Substantial edge tiltings or rotations of the four other tetrahedral (O1—O2) edges, identified as the most probable driving force of the high-pressure phase transition to triclinic symmetry (Wildner et al., 2021), are either forbidden or at least strongly hampered by the monoclinic symmetry prevailing also at very low temperatures [e.g. relative rotations of O1—O2 edges are <0.1° and therefore not shown in Fig. 4(d)].

Figure 5
Fragment of the crystal structure of kieserite (MgSO₄·H₂O) at 313 K, projected down the approximate c* direction, i.e. along [203]. On cooling, the black arrows show the direction of polyhedral rotations, red arrows indicate the components of the resulting positional shifts of the tetrahedral atoms in the plane of projection (see text).

The striking anisotropy of the thermal expansion tensor in the ac plane [Figs. 3(a) and 3(b)] can be correlated to the tetrahedral rotations described above. The sense of rotation on heating [indicated in Fig. 3(b) by black arrows] leads to, apart from comparable expansions of the a and c axes (Table 1), an opposite shift of neighboring octahedral–tetrahedral chains along the c axes [red arrows in Fig. 3(b)], resulting in a widening of the cell angle β (Fig. 2) and maximum expansion roughly along the long cell diagonal, while minimum expansion occurs near the [101] direction.

Although the anisotropy of thermal expansion in the ac plane can be readily explained, an attempt to elucidate reasons for the peculiar NTE behavior of the crystallographic b axis [Fig. 3(a), Table 1] needs to consider the mutual interactions of the various temperature-dependent structural changes observed in the present study. It appears that only a complex, cooperative effect involving polyhedral rotations, changes of the interpolyhedral M–O–S angles and shortening of the O3—H⋯O2 hydrogen bond length, can provoke this clear trend in contrast to the decrease in cell volume and other lattice directions on cooling. Fig. 5 illustrates the main contributing factors: firstly, the sense of major polyhedral rotations on cooling is shown, i.e. on the one hand the rotation of the SO₄ tetrahedron around its twofold symmetry axis [as discussed above; Figs. 3(b) and 4(d)], on the other hand a rotation of the MO₆ octahedron (point symmetry 1) approximately around its O3—O3 axis; secondly, it indicates the most relevant components of resulting positional shifts of the tetrahedral atoms in the plane of projection. Altogether, the SO₄ tetrahedron as a whole is shifted up along the b axis, thus involving an elongation of this axis on cooling, while at the same time the a axis, including the roughly parallel hydrogen bond, and to a lesser extent the c axis, are shortened. The comparatively weak NTE of the b axis in NiSO₄·H₂O (Table 1) can then be correlated, at least qualitatively, with the respective smallest temperature-dependent changes of the hydrogen bond lengths [Fig. 4(b)], of both M–O–S angles [Fig. 4(c)] and of the tetrahedral rotations [Fig. 4(d)] among the four title compounds.

3.5. Polyhedral thermal expansion versus compressibility

In analogy with the present low-temperature results, the decrease of the octahedral volume on pressure increase is also dominated by shortening of the longest M–O3 bonds to the water molecules, to a lesser extent also the M–O2 distances, while the M–O1 bonds are the stiffest and shorten the least [thus contributing to the high axial 〈M_a〉 values (Wildner et al., 2021, and references therein)]. When the octahedral volume thermal expansion values α_V,_oct (in the range 2.8–3.1 × 10⁻⁵ K⁻¹) are compared with the respective octahedral volume compression values β_V,_oct (1.1–1.4 × 10⁻⁶ bar⁻¹), we find a ratio α_V,oct/β_V,oct of ∼25 bar K⁻¹, i.e. for the MO₄(H₂O)₂ polyhedra a pressure change of approximately 25 bar offsets a temperature change of 1 K. Hence, judging from the influence of temperature and pressure on the octahedral units in kieserite-type compounds, cooling from RT to 15 K corresponds to a `thermal pressure effect' of ∼0.7 GPa, thus far below the magnitude of critical pressures mentioned earlier, and a further corroboration of the absence of structural phase transitions on cooling.

Across high-temperature and high-pressure studies on structure types of relevant rock-forming minerals, the ratio of α_V,oct/β_V,oct for most M²⁺O₆ octahedra is about three times higher than in kieserite, scattering between 65 and 90 bar K⁻¹ (e.g. Hazen & Prewitt, 1977 ; Hazen & Finger, 1982a,b ; Hazen et al., 2000 ). On the one hand, this difference can be attributed to the fact that α_poly increases with temperature: for high-temperature studies from RT up to 1000°C, Hazen & Prewitt (1977) found 〈α_V,_oct〉 ≃ 4.2 × 10⁻⁵ K⁻¹ (from axial α_oct ≃ 1.4 × 10⁻⁵ K⁻¹) for MgO₆ octahedra (and similar values for TM²⁺O₆ units). On the other hand, the compressibility β_V,oct of the MgO₆ octahedron in kieserite (Meusburger et al., 2020; Wildner et al., 2021) is approximately twice as large compared with the values usually found for MgO₆ units in oxides and silicates [where the polyhedral modulus K_oct ≃ 150 GPa (e.g. Hazen et al., 2000)], a discrepancy which can be reasonably explained by the presence of H₂O ligands and polyhedral connectivity through shared corners in the kieserite structure type.

4. Conclusions

The results for the in situ investigation of the crystal behavior of kieserite and three sulfate analog phases revealed that the structural topology remained unchanged within the experimental temperature range, i.e. down to 15 K. Neither the bond-length evolution nor the overall symmetry of the lattice is subject to a discontinuity that can be assigned to a phase transformation similar to that observed at high pressures for any of the four investigated M²⁺SO₄·H₂O (M²⁺ = Mg, Fe, Co, Ni) end-member phases. The monoclinic C2/c lattice of this so-called α-form shows a rather uniform volume expansivity with values for α_V between 3.3 and 4.7 × 10⁻⁵ K⁻¹, approximately following the inverse relationship to the molar volume and the size of the M²⁺ cation, respectively. On the other hand, the thermally induced lattice expansion is subject to a rather pronounced anisotropy, with an NTE along the [010] direction, and anisotropic positive eigenvalues for the strain tensor within the ac plane. The NTE effect can be related to cooperative polyhedral rotations associated with the chain motifs of tetrahedral SO₄ groups and octahedrally coordinated M²⁺ cations, which has also been observed for other sulfates exhibiting equivalent topological octahedral chain units.

As a major result of the present investigations, there is no evidence for a structural transition for any of the four investigated end-member compounds. This suggests that, for the kieserite-type solid solution series known to exist, there is no evidence for the occurrence of a low-temperature polymorphic transformation or dissociation, and phase stabilities are not affected even by the effect of cation substitution on temperature variations at ≤1 bar `atmospheric' pressure. In the context of evaluating structural aspects of phase-stability issues with respect to potentially changing hydration states, the experiments clearly show that there is no evidence for any changes with respect to the amount of water per formula unit.

The knowledge of phase relations and structural details at astrophysically relevant temperature conditions is an important fundament to derive, model and analyze other physical properties, e.g. by using density functional theory calculations. Based on the low-temperature structural behavior presented, ab initio calculations allow us to determine key thermodynamic properties of the phase of interest, such as heat of formation, enthalpy, entropy and the heat capacity (e.g. Deffrennes et al., 2019 ; Dinsdale et al., 2019 ; Bao et al., 2021 ). In turn, such as in the case of kieserite-type sulfate monohydrates, knowledge of these properties for end members allows us to extrapolate their values even for intermediate compositions, given the linear Vegard-type behavior along the solid solutions between kieserite and all isotypic TM end members investigated here (Bechtold & Wildner, 2016; Talla & Wildner, 2019; Talla et al., 2020). Knowledge of these parameters will contribute to future modeling of thermodynamic equilibria and stable surface mineral assemblages on various objects in our solar system even at very low temperatures. Last but not least, the absence of low-temperature structural phase transitions or dehydration effects on the one hand, and the smooth variation of stereochemical details with temperature on the other, also forms an important fundament to evaluate kieserite-related signals in remote-sensing spectroscopic data from orbiters at celestial bodies with lower surface temperatures than prevailing on Mars, e.g. on the surface on the icy Galilean moons.

Supporting information

Crystal structure: contains datablocks publication_text, MgSO4H2O_He_15K, MgSO4H2O_He_30K, MgSO4H2O_N2_113K, MgSO4H2O_N2_153K, MgSO4H2O_N2_193K, MgSO4H2O_N2_233K, MgSO4H2O_N2_273K, MgSO4H2O_N2_313K, FeSO4H2O_He_45K, FeSO4H2O_He_60K, FeSO4H2O_He_75K, FeSO4H2O_N2_113K, FeSO4H2O_N2_153K, FeSO4H2O_N2_193K, FeSO4H2O_N2_233K, FeSO4H2O_N2_273K, FeSO4H2O_N2_313K, CoSO4H2O_He_15K, CoSO4H2O_He_30K, CoSO4H2O_N2_113K, CoSO4H2O_N2_153K, CoSO4H2O_N2_193K, CoSO4H2O_N2_233K, CoSO4H2O_N2_273K, CoSO4H2O_N2_313K, NiSO4H2O_He_15K, NiSO4H2O_He_45K, NiSO4H2O_He_75K, NiSO4H2O_N2_113K, NiSO4H2O_N2_153K, NiSO4H2O_N2_193K, NiSO4H2O_N2_233K, NiSO4H2O_N2_273K, NiSO4H2O_N2_313K. DOI: https://doi.org/10.1107/S2052252521012720/lt5044sup1.cif

Supporting figures and table. DOI: https://doi.org/10.1107/S2052252521012720/lt5044sup2.pdf

Computing details top

Program(s) used to solve structure: SHELXT 2014/5 (Sheldrick, 2014) for MgSO4H2O_N2_233K. Program(s) used to refine structure: SHELXL2017/1 (Sheldrick, 2017) for MgSO4H2O_He_15K, MgSO4H2O_N2_113K, MgSO4H2O_N2_153K, MgSO4H2O_N2_193K, MgSO4H2O_N2_233K, MgSO4H2O_N2_273K, MgSO4H2O_N2_313K, FeSO4H2O_He_60K, FeSO4H2O_He_75K, FeSO4H2O_N2_113K, FeSO4H2O_N2_153K, FeSO4H2O_N2_193K, FeSO4H2O_N2_233K, FeSO4H2O_N2_273K, FeSO4H2O_N2_313K, CoSO4H2O_He_15K, CoSO4H2O_He_30K, CoSO4H2O_N2_113K, CoSO4H2O_N2_153K, CoSO4H2O_N2_193K, CoSO4H2O_N2_233K, CoSO4H2O_N2_273K, CoSO4H2O_N2_313K, NiSO4H2O_He_45K, NiSO4H2O_He_75K, NiSO4H2O_N2_113K, NiSO4H2O_N2_153K, NiSO4H2O_N2_193K, NiSO4H2O_N2_233K, NiSO4H2O_N2_273K, NiSO4H2O_N2_313K; SHELXL2018/3 (Sheldrick, 2018) for MgSO4H2O_He_30K, FeSO4H2O_He_45K, NiSO4H2O_He_15K.

(MgSO4H2O_He_15K) top

Crystal data top

H₂MgO₅S	Z = 4
M_r = 138.39	F(000) = 280
Monoclinic, C2/c	D_x = 2.597 Mg m⁻³
a = 6.8611 (6) Å	Mo Kα radiation, λ = 0.71073 Å
b = 7.6716 (6) Å	µ = 0.97 mm⁻¹
c = 7.6014 (7) Å	T = 15 K
β = 117.787 (12)°	0.38 × 0.30 × 0.06 mm
V = 353.97 (6) Å³

Data collection top

1215 measured reflections	θ_max = 29.2°, θ_min = 4.3°
422 independent reflections	h = −7→9
381 reflections with I > 2σ(I)	k = −8→9
R_int = 0.023	l = −9→8

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.023	w = 1/[σ²(F_o²) + (0.026P)² + 0.470P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.058	(Δ/σ)_max < 0.001
S = 1.11	Δρ_max = 0.41 e Å⁻³
422 reflections	Δρ_min = −0.50 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.077 (5)

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Mg	0.000000	0.500000	0.000000	0.0038 (3)
S	0.000000	0.15743 (8)	0.250000	0.0030 (2)
O1	0.17523 (19)	0.04823 (17)	0.39724 (17)	0.0049 (3)
O2	0.09598 (19)	0.27005 (17)	0.15141 (18)	0.0048 (3)
O3	0.000000	0.6334 (3)	0.250000	0.0049 (4)
H	0.101 (4)	0.700 (4)	0.288 (4)	0.021 (7)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mg	0.0035 (4)	0.0038 (5)	0.0049 (4)	0.0000 (3)	0.0025 (3)	0.0005 (3)
S	0.0030 (3)	0.0029 (4)	0.0037 (3)	0.000	0.0022 (2)	0.000
O1	0.0040 (6)	0.0042 (7)	0.0062 (6)	0.0010 (5)	0.0022 (5)	0.0011 (5)
O2	0.0042 (6)	0.0041 (7)	0.0069 (6)	0.0000 (5)	0.0034 (5)	0.0012 (5)
O3	0.0037 (9)	0.0040 (9)	0.0065 (9)	0.000	0.0020 (7)	0.000

Geometric parameters (Å, º) top

Mg—O1ⁱ	2.0223 (12)	O1—O2	2.3950 (17)
Mg—O1ⁱⁱ	2.0223 (12)	O1—O1^v	2.403 (2)
Mg—O2ⁱⁱⁱ	2.0405 (13)	O1—O2^v	2.4194 (17)
Mg—O2	2.0405 (13)	O1—O2^vi	2.7743 (17)
Mg—O3	2.1583 (9)	O1—O3^vii	2.9199 (16)
Mg—O3ⁱⁱⁱ	2.1583 (9)	O1—O2^viii	2.9681 (17)
Mg—O2ⁱ	3.4855 (13)	O1—O3^ix	2.9950 (13)
Mg—O2ⁱⁱ	3.4855 (13)	O1—O2^x	3.3121 (18)
Mg—O2^iv	3.4920 (12)	O1—O2^vii	3.3402 (18)
Mg—O2^v	3.4920 (12)	O1—O3^xi	3.402 (2)
Mg—O1^iv	3.8656 (13)	O2—O2^v	2.413 (2)
Mg—O1^v	3.8656 (13)	O2—O3^ix	2.7218 (14)
S—O1^v	1.4647 (13)	O2—O3ⁱⁱⁱ	2.9016 (13)
S—O1	1.4647 (13)	O2—O3	3.037 (2)
S—O2	1.4838 (12)	O3—H	0.80 (3)
S—O2^v	1.4839 (12)	O3—H^v	0.80 (3)

O1ⁱ—Mg—O1ⁱⁱ	180.0	S—O2—O3^ix	105.75 (7)
O1ⁱ—Mg—O2ⁱⁱⁱ	86.13 (5)	Mg—O2—O3^ix	120.51 (6)
O1ⁱⁱ—Mg—O2ⁱⁱⁱ	93.87 (5)	O1—O2—O3^ix	71.33 (5)
O1ⁱ—Mg—O2	93.87 (5)	O2^v—O2—O3^ix	127.57 (7)
O1ⁱⁱ—Mg—O2	86.13 (5)	O1^v—O2—O3^ix	112.53 (7)
O2ⁱⁱⁱ—Mg—O2	180.0	S—O2—O1ⁱⁱ	157.99 (8)
O1ⁱ—Mg—O3	88.54 (4)	Mg—O2—O1ⁱⁱ	46.66 (4)
O1ⁱⁱ—Mg—O3	91.46 (4)	O1—O2—O1ⁱⁱ	135.55 (5)
O2ⁱⁱⁱ—Mg—O3	87.38 (6)	O2^v—O2—O1ⁱⁱ	126.12 (4)
O2—Mg—O3	92.62 (6)	O1^v—O2—O1ⁱⁱ	164.44 (8)
O1ⁱ—Mg—O3ⁱⁱⁱ	91.46 (4)	O3^ix—O2—O1ⁱⁱ	76.47 (5)
O1ⁱⁱ—Mg—O3ⁱⁱⁱ	88.54 (4)	S—O2—O3ⁱⁱⁱ	138.00 (7)
O2ⁱⁱⁱ—Mg—O3ⁱⁱⁱ	92.62 (6)	Mg—O2—O3ⁱⁱⁱ	47.99 (4)
O2—Mg—O3ⁱⁱⁱ	87.38 (6)	O1—O2—O3ⁱⁱⁱ	149.27 (7)
O3—Mg—O3ⁱⁱⁱ	180.0	O2^v—O2—O3ⁱⁱⁱ	136.99 (7)
O1ⁱ—Mg—O2ⁱ	41.84 (4)	O1^v—O2—O3ⁱⁱⁱ	103.74 (6)
O1ⁱⁱ—Mg—O2ⁱ	138.16 (4)	O3^ix—O2—O3ⁱⁱⁱ	95.20 (4)
O2ⁱⁱⁱ—Mg—O2ⁱ	98.74 (2)	O1ⁱⁱ—O2—O3ⁱⁱⁱ	61.87 (5)
O2—Mg—O2ⁱ	81.26 (2)	S—O2—O1ⁱ	94.37 (6)
O3—Mg—O2ⁱ	128.66 (3)	Mg—O2—O1ⁱ	42.83 (3)
O3ⁱⁱⁱ—Mg—O2ⁱ	51.34 (3)	O1—O2—O1ⁱ	129.77 (7)
O1ⁱ—Mg—O2ⁱⁱ	138.16 (4)	O2^v—O2—O1ⁱ	75.96 (5)
O1ⁱⁱ—Mg—O2ⁱⁱ	41.84 (4)	O1^v—O2—O1ⁱ	77.61 (5)
O2ⁱⁱⁱ—Mg—O2ⁱⁱ	81.26 (2)	O3^ix—O2—O1ⁱ	156.46 (5)
O2—Mg—O2ⁱⁱ	98.74 (2)	O1ⁱⁱ—O2—O1ⁱ	89.49 (5)
O3—Mg—O2ⁱⁱ	51.34 (3)	O3ⁱⁱⁱ—O2—O1ⁱ	61.35 (4)
O3ⁱⁱⁱ—Mg—O2ⁱⁱ	128.66 (3)	S—O2—O3	102.21 (6)
O2ⁱ—Mg—O2ⁱⁱ	180.0	Mg—O2—O3	45.23 (3)
O1ⁱ—Mg—O2^iv	111.28 (4)	O1—O2—O3	117.13 (5)
O1ⁱⁱ—Mg—O2^iv	68.72 (4)	O2^v—O2—O3	66.60 (3)
O2ⁱⁱⁱ—Mg—O2^iv	42.33 (4)	O1^v—O2—O3	116.33 (5)
O2—Mg—O2^iv	137.67 (4)	O3^ix—O2—O3	126.56 (6)
O3—Mg—O2^iv	120.40 (5)	O1ⁱⁱ—O2—O3	61.85 (4)
O3ⁱⁱⁱ—Mg—O2^iv	59.60 (5)	O3ⁱⁱⁱ—O2—O3	93.22 (4)
O2ⁱ—Mg—O2^iv	95.04 (3)	O1ⁱ—O2—O3	58.17 (3)
O2ⁱⁱ—Mg—O2^iv	84.96 (3)	S—O2—O1^xii	95.60 (6)
O1ⁱ—Mg—O2^v	68.72 (4)	Mg—O2—O1^xii	113.95 (5)
O1ⁱⁱ—Mg—O2^v	111.28 (4)	O1—O2—O1^xii	83.80 (4)
O2ⁱⁱⁱ—Mg—O2^v	137.67 (4)	O2^v—O2—O1^xii	130.39 (4)
O2—Mg—O2^v	42.33 (4)	O1^v—O2—O1^xii	73.50 (5)
O3—Mg—O2^v	59.60 (5)	O3^ix—O2—O1^xii	56.88 (4)
O3ⁱⁱⁱ—Mg—O2^v	120.40 (5)	O1ⁱⁱ—O2—O1^xii	103.44 (5)
O2ⁱ—Mg—O2^v	84.96 (3)	O3ⁱⁱⁱ—O2—O1^xii	66.00 (5)
O2ⁱⁱ—Mg—O2^v	95.04 (3)	O1ⁱ—O2—O1^xii	109.93 (5)
O2^iv—Mg—O2^v	180.0	O3—O2—O1^xii	159.06 (5)
O1ⁱ—Mg—O1^iv	118.46 (5)	S—O2—O1^vii	80.27 (5)
O1ⁱⁱ—Mg—O1^iv	61.54 (5)	Mg—O2—O1^vii	95.28 (5)
O2ⁱⁱⁱ—Mg—O1^iv	32.85 (4)	O1—O2—O1^vii	70.62 (5)
O2—Mg—O1^iv	147.15 (4)	O2^v—O2—O1^vii	59.55 (5)
O3—Mg—O1^iv	83.14 (5)	O1^v—O2—O1^vii	114.22 (6)
O3ⁱⁱⁱ—Mg—O1^iv	96.86 (5)	O3^ix—O2—O1^vii	86.98 (4)
O2ⁱ—Mg—O1^iv	126.25 (3)	O1ⁱⁱ—O2—O1^vii	77.98 (4)
O2ⁱⁱ—Mg—O1^iv	53.75 (3)	O3ⁱⁱⁱ—O2—O1^vii	137.83 (6)
O2^iv—Mg—O1^iv	37.56 (3)	O1ⁱ—O2—O1^vii	108.74 (5)
O2^v—Mg—O1^iv	142.44 (3)	O3—O2—O1^vii	54.25 (3)
O1ⁱ—Mg—O1^v	61.54 (5)	O1^xii—O2—O1^vii	141.31 (4)
O1ⁱⁱ—Mg—O1^v	118.46 (5)	Mg—O3—Mg^v	123.40 (9)
O2ⁱⁱⁱ—Mg—O1^v	147.15 (4)	Mg—O3—O2^xiii	110.99 (3)
O2—Mg—O1^v	32.85 (4)	Mg^v—O3—O2^xiii	90.40 (3)
O3—Mg—O1^v	96.86 (5)	Mg—O3—O2ⁱⁱ	90.40 (3)
O3ⁱⁱⁱ—Mg—O1^v	83.14 (5)	Mg^v—O3—O2ⁱⁱ	110.99 (3)
O2ⁱ—Mg—O1^v	53.75 (3)	O2^xiii—O3—O2ⁱⁱ	134.69 (9)
O2ⁱⁱ—Mg—O1^v	126.25 (3)	Mg—O3—O2^xiv	162.51 (7)
O2^iv—Mg—O1^v	142.44 (3)	Mg^v—O3—O2^xiv	44.63 (3)
O2^v—Mg—O1^v	37.56 (3)	O2^xiii—O3—O2^xiv	83.91 (4)
O1^iv—Mg—O1^v	180.0	O2ⁱⁱ—O3—O2^xiv	84.80 (4)
O1^v—S—O1	110.23 (11)	Mg—O3—O2ⁱⁱⁱ	44.63 (3)
O1^v—S—O2	110.27 (6)	Mg^v—O3—O2ⁱⁱⁱ	162.51 (7)
O1—S—O2	108.63 (7)	O2^xiii—O3—O2ⁱⁱⁱ	84.80 (4)
O1^v—S—O2^v	108.63 (6)	O2ⁱⁱ—O3—O2ⁱⁱⁱ	83.91 (4)
O1—S—O2^v	110.27 (6)	O2^xiv—O3—O2ⁱⁱⁱ	150.42 (9)
O2—S—O2^v	108.78 (10)	Mg—O3—O1ⁱ	43.82 (3)
S—O1—Mg^vi	139.81 (8)	Mg^v—O3—O1ⁱ	105.61 (6)
S—O1—O2	35.95 (4)	O2^xiii—O3—O1ⁱ	71.80 (4)
Mg^vi—O1—O2	103.88 (6)	O2ⁱⁱ—O3—O1ⁱ	132.84 (4)
S—O1—O1^v	34.88 (5)	O2^xiv—O3—O1ⁱ	142.13 (4)
Mg^vi—O1—O1^v	143.48 (8)	O2ⁱⁱⁱ—O3—O1ⁱ	56.92 (3)
O2—O1—O1^v	60.56 (5)	Mg—O3—O1^vii	105.61 (6)
S—O1—O2^v	35.12 (4)	Mg^v—O3—O1^vii	43.82 (3)
Mg^vi—O1—O2^v	144.90 (7)	O2^xiii—O3—O1^vii	132.84 (4)
O2—O1—O2^v	60.15 (6)	O2ⁱⁱ—O3—O1^vii	71.80 (4)
O1^v—O1—O2^v	59.56 (5)	O2^xiv—O3—O1^vii	56.92 (3)
S—O1—O2^vi	130.69 (7)	O2ⁱⁱⁱ—O3—O1^vii	142.13 (4)
Mg^vi—O1—O2^vi	47.21 (4)	O1ⁱ—O3—O1^vii	123.00 (9)
O2—O1—O2^vi	112.29 (5)	Mg—O3—O1^xiii	122.07 (6)
O1^v—O1—O2^vi	104.98 (5)	Mg^v—O3—O1^xiii	42.45 (3)
O2^v—O1—O2^vi	164.44 (8)	O2^xiii—O3—O1^xiii	49.25 (3)
S—O1—O3^vii	167.91 (7)	O2ⁱⁱ—O3—O1^xiii	145.16 (4)
Mg^vi—O1—O3^vii	47.64 (3)	O2^xiv—O3—O1^xiii	60.42 (3)
O2—O1—O3^vii	148.65 (6)	O2ⁱⁱⁱ—O3—O1^xiii	127.23 (3)
O1^v—O1—O3^vii	149.24 (5)	O1ⁱ—O3—O1^xiii	81.77 (4)
O2^v—O1—O3^vii	132.79 (6)	O1^vii—O3—O1^xiii	86.27 (4)
O2^vi—O1—O3^vii	61.21 (4)	Mg—O3—O1ⁱⁱ	42.45 (3)
S—O1—O2^viii	115.57 (7)	Mg^v—O3—O1ⁱⁱ	122.07 (6)
Mg^vi—O1—O2^viii	43.31 (4)	O2^xiii—O3—O1ⁱⁱ	145.16 (4)
O2—O1—O2^viii	88.41 (5)	O2ⁱⁱ—O3—O1ⁱⁱ	49.25 (3)
O1^v—O1—O2^viii	148.60 (5)	O2^xiv—O3—O1ⁱⁱ	127.23 (3)
O2^v—O1—O2^viii	102.39 (5)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	60.42 (3)
O2^vi—O1—O2^viii	90.52 (5)	O1ⁱ—O3—O1ⁱⁱ	86.27 (4)
O3^vii—O1—O2^viii	62.10 (5)	O1^vii—O3—O1ⁱⁱ	81.77 (4)
S—O1—O3^ix	94.49 (6)	O1^xiii—O3—O1ⁱⁱ	154.80 (9)
Mg^vi—O1—O3^ix	46.09 (3)	Mg—O3—O2	42.15 (4)
O2—O1—O3^ix	59.42 (5)	Mg^v—O3—O2	82.60 (6)
O1^v—O1—O3^ix	104.33 (6)	O2^xiii—O3—O2	126.56 (6)
O2^v—O1—O3^ix	116.27 (6)	O2ⁱⁱ—O3—O2	96.39 (3)
O2^vi—O1—O3^ix	63.40 (5)	O2^xiv—O3—O2	121.65 (6)
O3^vii—O1—O3^ix	93.73 (4)	O2ⁱⁱⁱ—O3—O2	86.78 (4)
O2^viii—O1—O3^ix	58.23 (4)	O1ⁱ—O3—O2	59.73 (5)
S—O1—O2^x	124.60 (7)	O1^vii—O3—O2	68.18 (5)
Mg^vi—O1—O2^x	95.21 (5)	O1^xiii—O3—O2	100.18 (6)
O2—O1—O2^x	159.99 (7)	O1ⁱⁱ—O3—O2	54.76 (4)
O1^v—O1—O2^x	100.27 (5)	Mg—O3—O2^v	82.60 (6)
O2^v—O1—O2^x	106.50 (5)	Mg^v—O3—O2^v	42.15 (4)
O2^vi—O1—O2^x	76.56 (5)	O2^xiii—O3—O2^v	96.39 (3)
O3^vii—O1—O2^x	51.32 (4)	O2ⁱⁱ—O3—O2^v	126.56 (6)
O2^viii—O1—O2^x	109.93 (5)	O2^xiv—O3—O2^v	86.78 (4)
O3^ix—O1—O2^x	137.04 (6)	O2ⁱⁱⁱ—O3—O2^v	121.65 (6)
S—O1—O2^vii	111.81 (7)	O1ⁱ—O3—O2^v	68.18 (5)
Mg^vi—O1—O2^vii	76.94 (4)	O1^vii—O3—O2^v	59.73 (5)
O2—O1—O2^vii	109.38 (5)	O1^xiii—O3—O2^v	54.76 (4)
O1^v—O1—O2^vii	138.06 (6)	O1ⁱⁱ—O3—O2^v	100.18 (6)
O2^v—O1—O2^vii	79.81 (4)	O2—O3—O2^v	46.81 (5)
O2^vi—O1—O2^vii	115.71 (6)	Mg—O3—H	105.6 (18)
O3^vii—O1—O2^vii	57.58 (5)	Mg^v—O3—H	109.7 (19)
O2^viii—O1—O2^vii	44.49 (4)	O2^xiii—O3—H	117.0 (19)
O3^ix—O1—O2^vii	102.56 (4)	O2ⁱⁱ—O3—H	18.9 (19)
O2^x—O1—O2^vii	80.50 (3)	O2^xiv—O3—H	73.7 (18)
S—O1—O3^xi	104.20 (6)	O2ⁱⁱⁱ—O3—H	87.4 (19)
Mg^vi—O1—O3^xi	96.47 (5)	O1ⁱ—O3—H	143.3 (18)
O2—O1—O3^xi	119.42 (5)	O1^vii—O3—H	79.0 (19)
O1^v—O1—O3^xi	69.32 (2)	O1^xiii—O3—H	132.3 (18)
O2^v—O1—O3^xi	118.62 (5)	O1ⁱⁱ—O3—H	66.8 (19)
O2^vi—O1—O3^xi	51.07 (3)	O2—O3—H	115.2 (19)
O3^vii—O1—O3^xi	81.78 (4)	O2^v—O3—H	138.4 (19)
O2^viii—O1—O3^xi	137.81 (5)	Mg—O3—H^v	109.7 (19)
O3^ix—O1—O3^xi	106.95 (5)	Mg^v—O3—H^v	105.6 (18)
O2^x—O1—O3^xi	51.19 (3)	O2^xiii—O3—H^v	18.9 (19)
O2^vii—O1—O3^xi	130.78 (5)	O2ⁱⁱ—O3—H^v	117.0 (19)
S—O2—Mg	133.30 (7)	O2^xiv—O3—H^v	87.4 (19)
S—O2—O1	35.42 (4)	O2ⁱⁱⁱ—O3—H^v	73.7 (18)
Mg—O2—O1	161.91 (7)	O1ⁱ—O3—H^v	79.0 (19)
S—O2—O2^v	35.61 (5)	O1^vii—O3—H^v	143.3 (18)
Mg—O2—O2^v	102.96 (4)	O1^xiii—O3—H^v	66.8 (19)
O1—O2—O2^v	60.43 (5)	O1ⁱⁱ—O3—H^v	132.3 (18)
S—O2—O1^v	34.60 (4)	O2—O3—H^v	138.4 (19)
Mg—O2—O1^v	119.93 (6)	O2^v—O3—H^v	115.2 (19)
O1—O2—O1^v	59.88 (6)	H—O3—H^v	101 (4)
O2^v—O2—O1^v	59.42 (4)

O1^v—S—O1—Mg^vi	118.67 (13)	O1^v—S—O2—Mg	80.87 (11)
O2—S—O1—Mg^vi	−2.26 (14)	O1—S—O2—Mg	−158.22 (9)
O2^v—S—O1—Mg^vi	−121.39 (12)	O2^v—S—O2—Mg	−38.16 (7)
O1^v—S—O1—O2	120.93 (6)	O1^v—S—O2—O1	−120.90 (11)
O2^v—S—O1—O2	−119.13 (10)	O2^v—S—O2—O1	120.06 (6)
O2—S—O1—O1^v	−120.93 (6)	O1^v—S—O2—O2^v	119.04 (6)
O2^v—S—O1—O1^v	119.94 (6)	O1—S—O2—O2^v	−120.06 (6)
O1^v—S—O1—O2^v	−119.94 (6)	O1—S—O2—O1^v	120.90 (11)
O2—S—O1—O2^v	119.13 (10)	O2^v—S—O2—O1^v	−119.04 (6)
O1^v—S—O1—O2^vi	50.41 (7)	O1^v—S—O2—O3^ix	−106.99 (7)
O2—S—O1—O2^vi	−70.52 (10)	O1—S—O2—O3^ix	13.91 (8)
O2^v—S—O1—O2^vi	170.36 (10)	O2^v—S—O2—O3^ix	133.97 (7)
O1^v—S—O1—O3^vii	−118.5 (4)	O1^v—S—O2—O1ⁱⁱ	160.2 (2)
O2—S—O1—O3^vii	120.5 (4)	O1—S—O2—O1ⁱⁱ	−78.9 (2)
O2^v—S—O1—O3^vii	1.4 (4)	O2^v—S—O2—O1ⁱⁱ	41.15 (17)
O1^v—S—O1—O2^viii	165.53 (8)	O1^v—S—O2—O3ⁱⁱⁱ	10.00 (13)
O2—S—O1—O2^viii	44.60 (8)	O1—S—O2—O3ⁱⁱⁱ	130.91 (10)
O2^v—S—O1—O2^viii	−74.52 (9)	O2^v—S—O2—O3ⁱⁱⁱ	−109.03 (11)
O1^v—S—O1—O3^ix	108.75 (6)	O1^v—S—O2—O1ⁱ	60.68 (8)
O2—S—O1—O3^ix	−12.18 (8)	O1—S—O2—O1ⁱ	−178.42 (6)
O2^v—S—O1—O3^ix	−131.30 (7)	O2^v—S—O2—O1ⁱ	−58.36 (4)
O1^v—S—O1—O2^x	−52.35 (6)	O1^v—S—O2—O3	119.04 (6)
O2—S—O1—O2^x	−173.28 (7)	O1—S—O2—O3	−120.06 (6)
O2^v—S—O1—O2^x	67.59 (10)	O2^v—S—O2—O3	0.000 (1)
O1^v—S—O1—O2^vii	−145.79 (7)	O1^v—S—O2—O1^xii	−49.87 (8)
O2—S—O1—O2^vii	93.28 (7)	O1—S—O2—O1^xii	71.03 (6)
O2^v—S—O1—O2^vii	−25.85 (8)	O2^v—S—O2—O1^xii	−168.91 (6)
O1^v—S—O1—O3^xi	−0.002 (1)	O1^v—S—O2—O1^vii	168.97 (6)
O2—S—O1—O3^xi	−120.93 (6)	O1—S—O2—O1^vii	−70.13 (7)
O2^v—S—O1—O3^xi	119.94 (6)	O2^v—S—O2—O1^vii	49.94 (3)

Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) −x+1/2, y+1/2, −z+1/2; (iii) −x, −y+1, −z; (iv) x, −y+1, z−1/2; (v) −x, y, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) x, y−1, z; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱ	0.80 (3)	1.99 (2)	2.7218 (14)	154 (3)

Symmetry code: (ii) −x+1/2, y+1/2, −z+1/2.

(MgSO4H2O_He_30K) top

Crystal data top

H₂MgO₅S	V = 353.38 (9) Å³
M_r = 138.39	Z = 4
Monoclinic, C2/c	F(000) = 280
a = 6.8560 (9) Å	D_x = 2.601 Mg m⁻³
b = 7.6675 (8) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.6008 (10) Å	µ = 0.97 mm⁻¹
β = 117.821 (17)°	T = 30 K

Data collection top

1031 measured reflections	θ_max = 29.2°, θ_min = 4.3°
410 independent reflections	h = −7→9
352 reflections with I > 2σ(I)	k = −8→9
R_int = 0.071	l = −9→8

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.051	w = 1/[σ²(F_o²) + (0.078P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.127	(Δ/σ)_max < 0.001
S = 1.05	Δρ_max = 0.82 e Å⁻³
410 reflections	Δρ_min = −0.96 e Å⁻³
40 parameters	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.133 (18)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Mg	0.000000	0.500000	0.000000	0.0057 (5)
S	0.000000	0.15735 (13)	0.250000	0.0046 (5)
O1	0.1756 (3)	0.0480 (3)	0.3969 (3)	0.0073 (6)
O2	0.0959 (3)	0.2699 (3)	0.1514 (3)	0.0070 (6)
O3	0.000000	0.6338 (4)	0.250000	0.0062 (8)
H	0.094 (7)	0.690 (7)	0.284 (6)	0.013 (11)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mg	0.0047 (8)	0.0041 (9)	0.0093 (8)	−0.0002 (5)	0.0042 (6)	0.0002 (5)
S	0.0037 (7)	0.0021 (7)	0.0084 (7)	0.000	0.0032 (5)	0.000
O1	0.0060 (11)	0.0068 (13)	0.0096 (11)	−0.0001 (8)	0.0040 (9)	0.0012 (8)
O2	0.0049 (11)	0.0047 (12)	0.0123 (10)	0.0005 (8)	0.0047 (9)	0.0010 (8)
O3	0.0039 (16)	0.0050 (16)	0.0087 (16)	0.000	0.0023 (13)	0.000

Geometric parameters (Å, º) top

Mg—O1ⁱ	2.017 (2)	S—O1	1.465 (2)
Mg—O1ⁱⁱ	2.017 (2)	S—O1^iv	1.465 (2)
Mg—O2	2.040 (2)	S—O2	1.483 (2)
Mg—O2ⁱⁱⁱ	2.040 (2)	S—O2^iv	1.483 (2)
Mg—O3ⁱⁱⁱ	2.1596 (17)	O3—H	0.72 (4)
Mg—O3	2.1596 (17)	O3—H^iv	0.72 (4)

O1ⁱ—Mg—O1ⁱⁱ	180.0	O1—S—O1^iv	110.13 (19)
O1ⁱ—Mg—O2	93.90 (8)	O1—S—O2	108.54 (11)
O1ⁱⁱ—Mg—O2	86.10 (8)	O1^iv—S—O2	110.41 (11)
O1ⁱ—Mg—O2ⁱⁱⁱ	86.10 (8)	O1—S—O2^iv	110.41 (11)
O1ⁱⁱ—Mg—O2ⁱⁱⁱ	93.90 (8)	O1^iv—S—O2^iv	108.54 (11)
O2—Mg—O2ⁱⁱⁱ	180.00 (12)	O2—S—O2^iv	108.79 (18)
O1ⁱ—Mg—O3ⁱⁱⁱ	91.40 (7)	S—O1—Mg^v	139.96 (14)
O1ⁱⁱ—Mg—O3ⁱⁱⁱ	88.60 (7)	S—O2—Mg	133.34 (12)
O2—Mg—O3ⁱⁱⁱ	87.32 (10)	Mg—O3—Mg^iv	123.26 (16)
O2ⁱⁱⁱ—Mg—O3ⁱⁱⁱ	92.68 (10)	Mg—O3—H	103 (3)
O1ⁱ—Mg—O3	88.60 (7)	Mg^iv—O3—H	110 (3)
O1ⁱⁱ—Mg—O3	91.40 (7)	Mg—O3—H^iv	110 (3)
O2—Mg—O3	92.68 (10)	Mg^iv—O3—H^iv	103 (3)
O2ⁱⁱⁱ—Mg—O3	87.32 (10)	H—O3—H^iv	106 (8)
O3ⁱⁱⁱ—Mg—O3	180.0

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

(MgSO4H2O_N2_113K) top

Crystal data top

Fe₀H₂MgO₅S	V = 354.18 (9) Å³
M_r = 138.39	Z = 4
Monoclinic, C2/c	F(000) = 280
a = 6.8648 (10) Å	D_x = 2.595 Mg m⁻³
b = 7.6684 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.6055 (10) Å	µ = 0.97 mm⁻¹
β = 117.792 (10)°	T = 113 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.018
T_min = 0.691, T_max = 0.748	θ_max = 40.0°, θ_min = 4.3°
9851 measured reflections	h = −12→12
1097 independent reflections	k = −13→13
1054 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.015	w = 1/[σ²(F_o²) + (0.018P)² + 0.210P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.043	(Δ/σ)_max < 0.001
S = 1.21	Δρ_max = 0.46 e Å⁻³
1097 reflections	Δρ_min = −0.40 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0059 (19)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Mg	0.000000	0.500000	0.000000	0.00431 (6)
S	0.000000	0.15710 (2)	0.250000	0.00337 (5)
O1	0.17522 (7)	0.04770 (6)	0.39686 (6)	0.00648 (7)
O2	0.09574 (7)	0.26975 (5)	0.15109 (6)	0.00597 (7)
O3	0.000000	0.63384 (8)	0.250000	0.00572 (9)
H	0.106 (2)	0.6987 (18)	0.290 (2)	0.019 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mg	0.00388 (11)	0.00445 (11)	0.00431 (10)	−0.00022 (8)	0.00167 (8)	0.00014 (8)
S	0.00268 (7)	0.00342 (7)	0.00377 (7)	0.000	0.00131 (5)	0.000
O1	0.00418 (14)	0.00732 (15)	0.00704 (14)	0.00193 (11)	0.00186 (11)	0.00289 (11)
O2	0.00588 (15)	0.00573 (14)	0.00753 (14)	0.00023 (11)	0.00417 (12)	0.00206 (11)
O3	0.0051 (2)	0.00623 (19)	0.00593 (19)	0.000	0.00259 (16)	0.000

Geometric parameters (Å, º) top

Mg—O1ⁱ	2.0222 (5)	O1—O2	2.3958 (6)
Mg—O1ⁱⁱ	2.0222 (5)	O1—O1^v	2.4013 (9)
Mg—O2	2.0410 (5)	O1—O2^v	2.4206 (6)
Mg—O2ⁱⁱⁱ	2.0410 (5)	O1—O2^vi	2.7719 (6)
Mg—O3ⁱⁱⁱ	2.1607 (4)	O1—O3^vii	2.9220 (6)
Mg—O3	2.1607 (4)	O1—O2^viii	2.9710 (7)
Mg—O2ⁱ	3.4864 (6)	O1—O3^ix	2.9962 (6)
Mg—O2ⁱⁱ	3.4864 (6)	O1—O2^x	3.3084 (7)
Mg—O2^iv	3.4954 (5)	O1—O2^vii	3.3483 (7)
Mg—O2^v	3.4954 (5)	O1—O3^xi	3.3932 (8)
Mg—O1^iv	3.8693 (6)	O2—O2^v	2.4156 (9)
Mg—O1^v	3.8693 (6)	O2—O3^ix	2.7216 (6)
S—O1^v	1.4647 (5)	O2—O3ⁱⁱⁱ	2.9008 (6)
S—O1	1.4647 (5)	O2—O3	3.0420 (8)
S—O2^v	1.4849 (4)	O3—H	0.817 (13)
S—O2	1.4849 (4)	O3—H^v	0.817 (13)

O1ⁱ—Mg—O1ⁱⁱ	180.0	S—O2—O3^ix	105.80 (2)
O1ⁱ—Mg—O2	93.971 (18)	Mg—O2—O3^ix	120.40 (2)
O1ⁱⁱ—Mg—O2	86.029 (18)	O1—O2—O3^ix	71.352 (18)
O1ⁱ—Mg—O2ⁱⁱⁱ	86.029 (18)	O2^v—O2—O3^ix	127.49 (2)
O1ⁱⁱ—Mg—O2ⁱⁱⁱ	93.971 (18)	O1^v—O2—O3^ix	112.65 (2)
O2—Mg—O2ⁱⁱⁱ	180.0	S—O2—O1ⁱⁱ	157.85 (3)
O1ⁱ—Mg—O3ⁱⁱⁱ	91.440 (16)	Mg—O2—O1ⁱⁱ	46.701 (14)
O1ⁱⁱ—Mg—O3ⁱⁱⁱ	88.560 (16)	O1—O2—O1ⁱⁱ	135.43 (2)
O2—Mg—O3ⁱⁱⁱ	87.27 (2)	O2^v—O2—O1ⁱⁱ	126.067 (15)
O2ⁱⁱⁱ—Mg—O3ⁱⁱⁱ	92.73 (2)	O1^v—O2—O1ⁱⁱ	164.64 (3)
O1ⁱ—Mg—O3	88.560 (15)	O3^ix—O2—O1ⁱⁱ	76.29 (2)
O1ⁱⁱ—Mg—O3	91.440 (15)	S—O2—O3ⁱⁱⁱ	138.09 (2)
O2—Mg—O3	92.73 (2)	Mg—O2—O3ⁱⁱⁱ	48.074 (14)
O2ⁱⁱⁱ—Mg—O3	87.27 (2)	O1—O2—O3ⁱⁱⁱ	149.22 (2)
O3ⁱⁱⁱ—Mg—O3	180.0	O2^v—O2—O3ⁱⁱⁱ	137.11 (3)
O1ⁱ—Mg—O2ⁱ	41.844 (15)	O1^v—O2—O3ⁱⁱⁱ	103.85 (2)
O1ⁱⁱ—Mg—O2ⁱ	138.156 (15)	O3^ix—O2—O3ⁱⁱⁱ	95.170 (17)
O2—Mg—O2ⁱ	81.277 (12)	O1ⁱⁱ—O2—O3ⁱⁱⁱ	61.959 (16)
O2ⁱⁱⁱ—Mg—O2ⁱ	98.724 (12)	S—O2—O1ⁱ	94.51 (2)
O3ⁱⁱⁱ—Mg—O2ⁱ	51.318 (12)	Mg—O2—O1ⁱ	42.766 (12)
O3—Mg—O2ⁱ	128.682 (12)	O1—O2—O1ⁱ	129.89 (2)
O1ⁱ—Mg—O2ⁱⁱ	138.156 (15)	O2^v—O2—O1ⁱ	76.09 (2)
O1ⁱⁱ—Mg—O2ⁱⁱ	41.844 (15)	O1^v—O2—O1ⁱ	77.77 (2)
O2—Mg—O2ⁱⁱ	98.723 (13)	O3^ix—O2—O1ⁱ	156.416 (19)
O2ⁱⁱⁱ—Mg—O2ⁱⁱ	81.276 (13)	O1ⁱⁱ—O2—O1ⁱ	89.467 (19)
O3ⁱⁱⁱ—Mg—O2ⁱⁱ	128.683 (12)	O3ⁱⁱⁱ—O2—O1ⁱ	61.350 (15)
O3—Mg—O2ⁱⁱ	51.317 (12)	S—O2—O3	102.18 (2)
O2ⁱ—Mg—O2ⁱⁱ	180.0	Mg—O2—O3	45.192 (11)
O1ⁱ—Mg—O2^iv	111.129 (17)	O1—O2—O3	117.14 (2)
O1ⁱⁱ—Mg—O2^iv	68.871 (17)	O2^v—O2—O3	66.607 (9)
O2—Mg—O2^iv	137.670 (16)	O1^v—O2—O3	116.32 (2)
O2ⁱⁱⁱ—Mg—O2^iv	42.330 (16)	O3^ix—O2—O3	126.38 (2)
O3ⁱⁱⁱ—Mg—O2^iv	59.650 (17)	O1ⁱⁱ—O2—O3	61.836 (15)
O3—Mg—O2^iv	120.350 (18)	O3ⁱⁱⁱ—O2—O3	93.266 (15)
O2ⁱ—Mg—O2^iv	94.967 (14)	O1ⁱ—O2—O3	58.135 (12)
O2ⁱⁱ—Mg—O2^iv	85.033 (15)	S—O2—O1^xii	95.77 (2)
O1ⁱ—Mg—O2^v	68.871 (17)	Mg—O2—O1^xii	113.89 (2)
O1ⁱⁱ—Mg—O2^v	111.129 (17)	O1—O2—O1^xii	83.881 (16)
O2—Mg—O2^v	42.330 (16)	O2^v—O2—O1^xii	130.533 (13)
O2ⁱⁱⁱ—Mg—O2^v	137.670 (16)	O1^v—O2—O1^xii	73.67 (2)
O3ⁱⁱⁱ—Mg—O2^v	120.350 (18)	O3^ix—O2—O1^xii	56.975 (15)
O3—Mg—O2^v	59.650 (17)	O1ⁱⁱ—O2—O1^xii	103.335 (18)
O2ⁱ—Mg—O2^v	85.033 (14)	O3ⁱⁱⁱ—O2—O1^xii	65.870 (17)
O2ⁱⁱ—Mg—O2^v	94.967 (15)	O1ⁱ—O2—O1^xii	109.96 (2)
O2^iv—Mg—O2^v	180.000 (14)	O3—O2—O1^xii	158.960 (17)
O1ⁱ—Mg—O1^iv	118.310 (17)	S—O2—O1^vii	80.21 (2)
O1ⁱⁱ—Mg—O1^iv	61.690 (17)	Mg—O2—O1^vii	95.174 (19)
O2—Mg—O1^iv	147.210 (14)	O1—O2—O1^vii	70.67 (2)
O2ⁱⁱⁱ—Mg—O1^iv	32.789 (14)	O2^v—O2—O1^vii	59.462 (19)
O3ⁱⁱⁱ—Mg—O1^iv	96.883 (17)	O1^v—O2—O1^vii	114.13 (2)
O3—Mg—O1^iv	83.117 (17)	O3^ix—O2—O1^vii	86.913 (17)
O2ⁱ—Mg—O1^iv	126.151 (12)	O1ⁱⁱ—O2—O1^vii	77.877 (15)
O2ⁱⁱ—Mg—O1^iv	53.849 (12)	O3ⁱⁱⁱ—O2—O1^vii	137.81 (2)
O2^iv—Mg—O1^iv	37.536 (9)	O1ⁱ—O2—O1^vii	108.65 (2)
O2^v—Mg—O1^iv	142.464 (9)	O3—O2—O1^vii	54.164 (11)
O1ⁱ—Mg—O1^v	61.690 (17)	O1^xii—O2—O1^vii	141.376 (16)
O1ⁱⁱ—Mg—O1^v	118.310 (17)	Mg—O3—Mg^v	123.28 (3)
O2—Mg—O1^v	32.790 (14)	Mg—O3—O2ⁱⁱ	90.386 (12)
O2ⁱⁱⁱ—Mg—O1^v	147.211 (15)	Mg^v—O3—O2ⁱⁱ	110.919 (14)
O3ⁱⁱⁱ—Mg—O1^v	83.117 (17)	Mg—O3—O2^xiii	110.920 (14)
O3—Mg—O1^v	96.883 (17)	Mg^v—O3—O2^xiii	90.386 (13)
O2ⁱ—Mg—O1^v	53.849 (12)	O2ⁱⁱ—O3—O2^xiii	134.97 (3)
O2ⁱⁱ—Mg—O1^v	126.151 (11)	Mg—O3—O2^xiv	162.46 (2)
O2^iv—Mg—O1^v	142.464 (9)	Mg^v—O3—O2^xiv	44.653 (11)
O2^v—Mg—O1^v	37.536 (9)	O2ⁱⁱ—O3—O2^xiv	84.830 (17)
O1^iv—Mg—O1^v	180.0	O2^xiii—O3—O2^xiv	83.966 (16)
O1^v—S—O1	110.12 (4)	Mg—O3—O2ⁱⁱⁱ	44.653 (11)
O1^v—S—O2^v	108.63 (2)	Mg^v—O3—O2ⁱⁱⁱ	162.46 (2)
O1—S—O2^v	110.30 (3)	O2ⁱⁱ—O3—O2ⁱⁱⁱ	83.967 (16)
O1^v—S—O2	110.30 (3)	O2^xiii—O3—O2ⁱⁱⁱ	84.831 (17)
O1—S—O2	108.63 (2)	O2^xiv—O3—O2ⁱⁱⁱ	150.47 (3)
O2^v—S—O2	108.85 (4)	Mg—O3—O1ⁱ	43.775 (13)
S—O1—Mg^vi	139.84 (3)	Mg^v—O3—O1ⁱ	105.63 (2)
S—O1—O2	35.967 (15)	O2ⁱⁱ—O3—O1ⁱ	132.782 (14)
Mg^vi—O1—O2	103.89 (2)	O2^xiii—O3—O1ⁱ	71.680 (16)
S—O1—O1^v	34.942 (19)	O2^xiv—O3—O1ⁱ	142.154 (15)
Mg^vi—O1—O1^v	143.71 (3)	O2ⁱⁱⁱ—O3—O1ⁱ	56.853 (14)
O2—O1—O1^v	60.609 (18)	Mg—O3—O1^vii	105.63 (2)
S—O1—O2^v	35.123 (15)	Mg^v—O3—O1^vii	43.775 (12)
Mg^vi—O1—O2^v	144.73 (2)	O2ⁱⁱ—O3—O1^vii	71.680 (16)
O2—O1—O2^v	60.20 (2)	O2^xiii—O3—O1^vii	132.781 (14)
O1^v—O1—O2^v	59.583 (18)	O2^xiv—O3—O1^vii	56.853 (15)
S—O1—O2^vi	130.89 (3)	O2ⁱⁱⁱ—O3—O1^vii	142.153 (15)
Mg^vi—O1—O2^vi	47.271 (13)	O1ⁱ—O3—O1^vii	123.10 (3)
O2—O1—O2^vi	112.375 (18)	Mg—O3—O1^xiii	121.92 (2)
O1^v—O1—O2^vi	105.15 (2)	Mg^v—O3—O1^xiii	42.431 (10)
O2^v—O1—O2^vi	164.64 (3)	O2ⁱⁱ—O3—O1^xiii	145.237 (15)
S—O1—O3^vii	167.73 (3)	O2^xiii—O3—O1^xiii	49.256 (14)
Mg^vi—O1—O3^vii	47.665 (12)	O2^xiv—O3—O1^xiii	60.479 (15)
O2—O1—O3^vii	148.68 (2)	O2ⁱⁱⁱ—O3—O1^xiii	127.238 (15)
O1^v—O1—O3^vii	149.226 (17)	O1ⁱ—O3—O1^xiii	81.727 (16)
O2^v—O1—O3^vii	132.61 (2)	O1^vii—O3—O1^xiii	86.206 (18)
O2^vi—O1—O3^vii	61.189 (16)	Mg—O3—O1ⁱⁱ	42.431 (10)
S—O1—O2^viii	115.45 (3)	Mg^v—O3—O1ⁱⁱ	121.92 (2)
Mg^vi—O1—O2^viii	43.263 (14)	O2ⁱⁱ—O3—O1ⁱⁱ	49.257 (14)
O2—O1—O2^viii	88.372 (19)	O2^xiii—O3—O1ⁱⁱ	145.237 (15)
O1^v—O1—O2^viii	148.583 (17)	O2^xiv—O3—O1ⁱⁱ	127.238 (15)
O2^v—O1—O2^viii	102.23 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	60.479 (14)
O2^vi—O1—O2^viii	90.534 (19)	O1ⁱ—O3—O1ⁱⁱ	86.206 (18)
O3^vii—O1—O2^viii	62.151 (18)	O1^vii—O3—O1ⁱⁱ	81.727 (16)
S—O1—O3^ix	94.51 (2)	O1^xiii—O3—O1ⁱⁱ	154.53 (3)
Mg^vi—O1—O3^ix	46.130 (13)	Mg—O3—O2	42.081 (13)
O2—O1—O3^ix	59.391 (17)	Mg^v—O3—O2	82.55 (2)
O1^v—O1—O3^ix	104.48 (3)	O2ⁱⁱ—O3—O2	96.303 (13)
O2^v—O1—O3^ix	116.22 (2)	O2^xiii—O3—O2	126.38 (2)
O2^vi—O1—O3^ix	63.519 (18)	O2^xiv—O3—O2	121.658 (18)
O3^vii—O1—O3^ix	93.795 (18)	O2ⁱⁱⁱ—O3—O2	86.734 (15)
O2^viii—O1—O3^ix	58.171 (15)	O1ⁱ—O3—O2	59.714 (16)
S—O1—O2^x	124.51 (2)	O1^vii—O3—O2	68.272 (17)
Mg^vi—O1—O2^x	95.318 (18)	O1^xiii—O3—O2	100.02 (2)
O2—O1—O2^x	159.93 (2)	O1ⁱⁱ—O3—O2	54.646 (13)
O1^v—O1—O2^x	100.196 (19)	Mg—O3—O2^v	82.55 (2)
O2^v—O1—O2^x	106.33 (2)	Mg^v—O3—O2^v	42.081 (13)
O2^vi—O1—O2^x	76.666 (18)	O2ⁱⁱ—O3—O2^v	126.38 (2)
O3^vii—O1—O2^x	51.346 (14)	O2^xiii—O3—O2^v	96.303 (13)
O2^viii—O1—O2^x	109.96 (2)	O2^xiv—O3—O2^v	86.734 (15)
O3^ix—O1—O2^x	137.244 (19)	O2ⁱⁱⁱ—O3—O2^v	121.658 (18)
S—O1—O2^vii	111.66 (2)	O1ⁱ—O3—O2^v	68.272 (18)
Mg^vi—O1—O2^vii	76.842 (18)	O1^vii—O3—O2^v	59.714 (16)
O2—O1—O2^vii	109.33 (2)	O1^xiii—O3—O2^v	54.646 (13)
O1^v—O1—O2^vii	137.93 (2)	O1ⁱⁱ—O3—O2^v	100.02 (2)
O2^v—O1—O2^vii	79.664 (17)	O2—O3—O2^v	46.786 (19)
O2^vi—O1—O2^vii	115.66 (2)	Mg—O3—H	104.3 (10)
O3^vii—O1—O2^vii	57.564 (17)	Mg^v—O3—H	109.3 (10)
O2^viii—O1—O2^vii	44.450 (16)	O2ⁱⁱ—O3—H	16.9 (10)
O3^ix—O1—O2^vii	102.462 (18)	O2^xiii—O3—H	119.4 (10)
O2^x—O1—O2^vii	80.445 (14)	O2^xiv—O3—H	74.4 (10)
S—O1—O3^xi	104.22 (2)	O2ⁱⁱⁱ—O3—H	87.6 (10)
Mg^vi—O1—O3^xi	96.663 (16)	O1ⁱ—O3—H	142.9 (10)
O2—O1—O3^xi	119.41 (2)	O1^vii—O3—H	77.4 (10)
O1^v—O1—O3^xi	69.278 (9)	O1^xiii—O3—H	133.6 (10)
O2^v—O1—O3^xi	118.61 (2)	O1ⁱⁱ—O3—H	65.1 (10)
O2^vi—O1—O3^xi	51.189 (14)	O2—O3—H	113.0 (10)
O3^vii—O1—O3^xi	81.862 (15)	O2^v—O3—H	136.6 (10)
O2^viii—O1—O3^xi	137.961 (16)	Mg—O3—H^v	109.3 (10)
O3^ix—O1—O3^xi	107.138 (17)	Mg^v—O3—H^v	104.3 (10)
O2^x—O1—O3^xi	51.278 (12)	O2ⁱⁱ—O3—H^v	119.4 (10)
O2^vii—O1—O3^xi	130.824 (15)	O2^xiii—O3—H^v	16.9 (10)
S—O2—Mg	133.32 (3)	O2^xiv—O3—H^v	87.6 (10)
S—O2—O1	35.403 (15)	O2ⁱⁱⁱ—O3—H^v	74.4 (10)
Mg—O2—O1	161.90 (2)	O1ⁱ—O3—H^v	77.4 (10)
S—O2—O2^v	35.573 (18)	O1^vii—O3—H^v	142.9 (10)
Mg—O2—O2^v	102.990 (16)	O1^xiii—O3—H^v	65.1 (10)
O1—O2—O2^v	60.409 (17)	O1ⁱⁱ—O3—H^v	133.6 (10)
S—O2—O1^v	34.577 (15)	O2—O3—H^v	136.6 (10)
Mg—O2—O1^v	120.04 (2)	O2^v—O3—H^v	113.0 (10)
O1—O2—O1^v	59.81 (2)	H—O3—H^v	104.9 (19)
O2^v—O2—O1^v	59.391 (17)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱ	0.817 (13)	1.955 (13)	2.7216 (6)	156.1 (13)

Symmetry code: (ii) −x+1/2, y+1/2, −z+1/2.

(MgSO4H2O_N2_153K) top

Crystal data top

Fe₀H₂MgO₅S	V = 354.35 (9) Å³
M_r = 138.39	Z = 4
Monoclinic, C2/c	F(000) = 280
a = 6.8717 (10) Å	D_x = 2.594 Mg m⁻³
b = 7.6629 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.6098 (10) Å	µ = 0.97 mm⁻¹
β = 117.833 (10)°	T = 153 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.019
T_min = 0.691, T_max = 0.748	θ_max = 40.0°, θ_min = 4.2°
9918 measured reflections	h = −12→12
1098 independent reflections	k = −13→13
1049 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.015	w = 1/[σ²(F_o²) + (0.019P)² + 0.180P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.044	(Δ/σ)_max < 0.001
S = 1.23	Δρ_max = 0.48 e Å⁻³
1098 reflections	Δρ_min = −0.41 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.005 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Mg	0.000000	0.500000	0.000000	0.00490 (6)
S	0.000000	0.15678 (2)	0.250000	0.00394 (5)
O1	0.17528 (7)	0.04724 (6)	0.39649 (6)	0.00764 (7)
O2	0.09519 (7)	0.26939 (5)	0.15082 (6)	0.00695 (7)
O3	0.000000	0.63402 (8)	0.250000	0.00651 (9)
H	0.105 (2)	0.6999 (18)	0.290 (2)	0.019 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mg	0.00441 (11)	0.00511 (11)	0.00489 (11)	−0.00030 (8)	0.00194 (8)	0.00018 (8)
S	0.00310 (7)	0.00392 (7)	0.00449 (7)	0.000	0.00152 (5)	0.000
O1	0.00485 (14)	0.00865 (15)	0.00845 (15)	0.00234 (11)	0.00228 (12)	0.00359 (12)
O2	0.00680 (15)	0.00652 (14)	0.00900 (15)	0.00050 (11)	0.00491 (12)	0.00257 (11)
O3	0.0059 (2)	0.0072 (2)	0.0065 (2)	0.000	0.00297 (16)	0.000

Geometric parameters (Å, º) top

Mg—O1ⁱ	2.0222 (5)	O1—O2	2.3948 (6)
Mg—O1ⁱⁱ	2.0222 (5)	O1—O1^v	2.3997 (9)
Mg—O2ⁱⁱⁱ	2.0413 (5)	O1—O2^v	2.4201 (6)
Mg—O2	2.0413 (5)	O1—O2^vi	2.7714 (6)
Mg—O3ⁱⁱⁱ	2.1619 (4)	O1—O3^vii	2.9223 (6)
Mg—O3	2.1619 (4)	O1—O2^viii	2.9717 (7)
Mg—O2ⁱⁱ	3.4868 (6)	O1—O3^ix	2.9978 (6)
Mg—O2ⁱ	3.4868 (6)	O1—O2^x	3.3061 (7)
Mg—O2^iv	3.4978 (5)	O1—O2^vii	3.3549 (8)
Mg—O2^v	3.4978 (5)	O1—O3^xi	3.3862 (8)
Mg—O1^iv	3.8722 (6)	O2—O2^v	2.4154 (9)
Mg—O1^v	3.8722 (6)	O2—O3^ix	2.7246 (6)
S—O1	1.4643 (5)	O2—O3ⁱⁱⁱ	2.9011 (6)
S—O1^v	1.4643 (5)	O2—O3	3.0439 (8)
S—O2	1.4843 (4)	O3—H	0.817 (13)
S—O2^v	1.4843 (4)	O3—H^v	0.817 (13)

O1ⁱ—Mg—O1ⁱⁱ	180.0	S—O2—O3^ix	105.85 (2)
O1ⁱ—Mg—O2ⁱⁱⁱ	86.004 (19)	Mg—O2—O3^ix	120.20 (2)
O1ⁱⁱ—Mg—O2ⁱⁱⁱ	93.996 (19)	O1—O2—O3^ix	71.357 (19)
O1ⁱ—Mg—O2	93.996 (19)	O2^v—O2—O3^ix	127.43 (3)
O1ⁱⁱ—Mg—O2	86.004 (19)	O1^v—O2—O3^ix	112.78 (2)
O2ⁱⁱⁱ—Mg—O2	180.0	S—O2—O1ⁱⁱ	157.72 (3)
O1ⁱ—Mg—O3ⁱⁱⁱ	91.465 (16)	Mg—O2—O1ⁱⁱ	46.710 (15)
O1ⁱⁱ—Mg—O3ⁱⁱⁱ	88.535 (16)	O1—O2—O1ⁱⁱ	135.25 (2)
O2ⁱⁱⁱ—Mg—O3ⁱⁱⁱ	92.76 (2)	O2^v—O2—O1ⁱⁱ	126.040 (16)
O2—Mg—O3ⁱⁱⁱ	87.24 (2)	O1^v—O2—O1ⁱⁱ	164.83 (3)
O1ⁱ—Mg—O3	88.535 (16)	O3^ix—O2—O1ⁱⁱ	76.06 (2)
O1ⁱⁱ—Mg—O3	91.465 (16)	S—O2—O3ⁱⁱⁱ	138.28 (3)
O2ⁱⁱⁱ—Mg—O3	87.24 (2)	Mg—O2—O3ⁱⁱⁱ	48.104 (14)
O2—Mg—O3	92.76 (2)	O1—O2—O3ⁱⁱⁱ	149.20 (2)
O3ⁱⁱⁱ—Mg—O3	180.0	O2^v—O2—O3ⁱⁱⁱ	137.31 (3)
O1ⁱ—Mg—O2ⁱⁱ	138.196 (15)	O1^v—O2—O3ⁱⁱⁱ	104.04 (2)
O1ⁱⁱ—Mg—O2ⁱⁱ	41.804 (15)	O3^ix—O2—O3ⁱⁱⁱ	95.062 (17)
O2ⁱⁱⁱ—Mg—O2ⁱⁱ	81.266 (13)	O1ⁱⁱ—O2—O3ⁱⁱⁱ	61.968 (17)
O2—Mg—O2ⁱⁱ	98.734 (12)	S—O2—O1ⁱ	94.68 (2)
O3ⁱⁱⁱ—Mg—O2ⁱⁱ	128.613 (12)	Mg—O2—O1ⁱ	42.751 (12)
O3—Mg—O2ⁱⁱ	51.387 (12)	O1—O2—O1ⁱ	130.08 (2)
O1ⁱ—Mg—O2ⁱ	41.805 (15)	O2^v—O2—O1ⁱ	76.26 (2)
O1ⁱⁱ—Mg—O2ⁱ	138.195 (15)	O1^v—O2—O1ⁱ	77.93 (2)
O2ⁱⁱⁱ—Mg—O2ⁱ	98.734 (13)	O3^ix—O2—O1ⁱ	156.311 (19)
O2—Mg—O2ⁱ	81.266 (13)	O1ⁱⁱ—O2—O1ⁱ	89.461 (19)
O3ⁱⁱⁱ—Mg—O2ⁱ	51.387 (12)	O3ⁱⁱⁱ—O2—O1ⁱ	61.374 (15)
O3—Mg—O2ⁱ	128.614 (12)	S—O2—O3	102.17 (2)
O2ⁱⁱ—Mg—O2ⁱ	180.0	Mg—O2—O3	45.188 (12)
O1ⁱ—Mg—O2^iv	110.994 (18)	O1—O2—O3	117.17 (2)
O1ⁱⁱ—Mg—O2^iv	69.006 (17)	O2^v—O2—O3	66.625 (10)
O2ⁱⁱⁱ—Mg—O2^iv	42.269 (16)	O1^v—O2—O3	116.33 (2)
O2—Mg—O2^iv	137.731 (17)	O3^ix—O2—O3	126.20 (2)
O3ⁱⁱⁱ—Mg—O2^iv	59.645 (18)	O1ⁱⁱ—O2—O3	61.851 (16)
O3—Mg—O2^iv	120.354 (18)	O3ⁱⁱⁱ—O2—O3	93.292 (15)
O2ⁱⁱ—Mg—O2^iv	85.078 (15)	O1ⁱ—O2—O3	58.112 (13)
O2ⁱ—Mg—O2^iv	94.922 (14)	S—O2—O1^xii	95.99 (2)
O1ⁱ—Mg—O2^v	69.006 (18)	Mg—O2—O1^xii	113.79 (2)
O1ⁱⁱ—Mg—O2^v	110.994 (17)	O1—O2—O1^xii	83.969 (16)
O2ⁱⁱⁱ—Mg—O2^v	137.731 (16)	O2^v—O2—O1^xii	130.739 (13)
O2—Mg—O2^v	42.269 (16)	O1^v—O2—O1^xii	73.91 (2)
O3ⁱⁱⁱ—Mg—O2^v	120.355 (17)	O3^ix—O2—O1^xii	56.993 (15)
O3—Mg—O2^v	59.646 (18)	O1ⁱⁱ—O2—O1^xii	103.143 (19)
O2ⁱⁱ—Mg—O2^v	94.922 (15)	O3ⁱⁱⁱ—O2—O1^xii	65.745 (18)
O2ⁱ—Mg—O2^v	85.078 (15)	O1ⁱ—O2—O1^xii	110.01 (2)
O2^iv—Mg—O2^v	180.0	O3—O2—O1^xii	158.842 (17)
O1ⁱ—Mg—O1^iv	118.204 (17)	S—O2—O1^vii	80.15 (2)
O1ⁱⁱ—Mg—O1^iv	61.796 (17)	Mg—O2—O1^vii	95.069 (19)
O2ⁱⁱⁱ—Mg—O1^iv	32.694 (15)	O1—O2—O1^vii	70.71 (2)
O2—Mg—O1^iv	147.306 (15)	O2^v—O2—O1^vii	59.37 (2)
O3ⁱⁱⁱ—Mg—O1^iv	96.824 (17)	O1^v—O2—O1^vii	114.05 (2)
O3—Mg—O1^iv	83.176 (17)	O3^ix—O2—O1^vii	86.865 (18)
O2ⁱⁱ—Mg—O1^iv	53.936 (12)	O1ⁱⁱ—O2—O1^vii	77.784 (15)
O2ⁱ—Mg—O1^iv	126.064 (12)	O3ⁱⁱⁱ—O2—O1^vii	137.72 (2)
O2^iv—Mg—O1^iv	37.491 (9)	O1ⁱ—O2—O1^vii	108.59 (2)
O2^v—Mg—O1^iv	142.509 (9)	O3—O2—O1^vii	54.083 (11)
O1ⁱ—Mg—O1^v	61.796 (17)	O1^xii—O2—O1^vii	141.399 (17)
O1ⁱⁱ—Mg—O1^v	118.204 (17)	Mg—O3—Mg^v	123.28 (3)
O2ⁱⁱⁱ—Mg—O1^v	147.306 (15)	Mg—O3—O2^xiii	110.889 (14)
O2—Mg—O1^v	32.694 (15)	Mg^v—O3—O2^xiii	90.296 (12)
O3ⁱⁱⁱ—Mg—O1^v	83.176 (17)	Mg—O3—O2ⁱⁱ	90.295 (13)
O3—Mg—O1^v	96.824 (17)	Mg^v—O3—O2ⁱⁱ	110.890 (14)
O2ⁱⁱ—Mg—O1^v	126.064 (12)	O2^xiii—O3—O2ⁱⁱ	135.24 (3)
O2ⁱ—Mg—O1^v	53.936 (12)	Mg—O3—O2^xiv	162.51 (2)
O2^iv—Mg—O1^v	142.509 (9)	Mg^v—O3—O2^xiv	44.654 (11)
O2^v—Mg—O1^v	37.491 (9)	O2^xiii—O3—O2^xiv	83.914 (17)
O1^iv—Mg—O1^v	180.0	O2ⁱⁱ—O3—O2^xiv	84.938 (17)
O1—S—O1^v	110.05 (4)	Mg—O3—O2ⁱⁱⁱ	44.654 (11)
O1—S—O2	108.62 (3)	Mg^v—O3—O2ⁱⁱⁱ	162.51 (2)
O1^v—S—O2	110.32 (3)	O2^xiii—O3—O2ⁱⁱⁱ	84.937 (18)
O1—S—O2^v	110.32 (3)	O2ⁱⁱ—O3—O2ⁱⁱⁱ	83.914 (16)
O1^v—S—O2^v	108.62 (3)	O2^xiv—O3—O2ⁱⁱⁱ	150.44 (3)
O2—S—O2^v	108.91 (4)	Mg—O3—O1ⁱ	43.770 (13)
S—O1—Mg^vi	139.91 (3)	Mg^v—O3—O1ⁱ	105.70 (2)
S—O1—O2	35.971 (16)	O2^xiii—O3—O1ⁱ	71.575 (17)
Mg^vi—O1—O2	103.94 (2)	O2ⁱⁱ—O3—O1ⁱ	132.687 (14)
S—O1—O1^v	34.976 (19)	O2^xiv—O3—O1ⁱ	142.144 (16)
Mg^vi—O1—O1^v	143.94 (3)	O2ⁱⁱⁱ—O3—O1ⁱ	56.837 (15)
O2—O1—O1^v	60.632 (19)	Mg—O3—O1^vii	105.70 (2)
S—O1—O2^v	35.110 (16)	Mg^v—O3—O1^vii	43.770 (13)
Mg^vi—O1—O2^v	144.59 (2)	O2^xiii—O3—O1^vii	132.687 (15)
O2—O1—O2^v	60.22 (2)	O2ⁱⁱ—O3—O1^vii	71.575 (16)
O1^v—O1—O2^v	59.584 (18)	O2^xiv—O3—O1^vii	56.837 (15)
S—O1—O2^vi	131.09 (3)	O2ⁱⁱⁱ—O3—O1^vii	142.144 (16)
Mg^vi—O1—O2^vi	47.286 (13)	O1ⁱ—O3—O1^vii	123.24 (3)
O2—O1—O2^vi	112.457 (19)	Mg—O3—O1^xiii	121.85 (2)
O1^v—O1—O2^vi	105.34 (2)	Mg^v—O3—O1^xiii	42.403 (10)
O2^v—O1—O2^vi	164.83 (3)	O2^xiii—O3—O1^xiii	49.196 (14)
S—O1—O3^vii	167.53 (3)	O2ⁱⁱ—O3—O1^xiii	145.326 (15)
Mg^vi—O1—O3^vii	47.694 (12)	O2^xiv—O3—O1^xiii	60.476 (15)
O2—O1—O3^vii	148.75 (2)	O2ⁱⁱⁱ—O3—O1^xiii	127.299 (15)
O1^v—O1—O3^vii	149.214 (17)	O1ⁱ—O3—O1^xiii	81.713 (16)
O2^v—O1—O3^vii	132.42 (2)	O1^vii—O3—O1^xiii	86.173 (18)
O2^vi—O1—O3^vii	61.195 (16)	Mg—O3—O1ⁱⁱ	42.403 (10)
S—O1—O2^viii	115.35 (3)	Mg^v—O3—O1ⁱⁱ	121.85 (2)
Mg^vi—O1—O2^viii	43.253 (14)	O2^xiii—O3—O1ⁱⁱ	145.325 (15)
O2—O1—O2^viii	88.377 (19)	O2ⁱⁱ—O3—O1ⁱⁱ	49.195 (14)
O1^v—O1—O2^viii	148.579 (17)	O2^xiv—O3—O1ⁱⁱ	127.299 (15)
O2^v—O1—O2^viii	102.07 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	60.476 (15)
O2^vi—O1—O2^viii	90.539 (19)	O1ⁱ—O3—O1ⁱⁱ	86.173 (18)
O3^vii—O1—O2^viii	62.181 (19)	O1^vii—O3—O1ⁱⁱ	81.713 (16)
S—O1—O3^ix	94.60 (2)	O1^xiii—O3—O1ⁱⁱ	154.37 (3)
Mg^vi—O1—O3^ix	46.133 (13)	Mg—O3—O2^v	82.56 (2)
O2—O1—O3^ix	59.449 (18)	Mg^v—O3—O2^v	42.053 (13)
O1^v—O1—O3^ix	104.66 (3)	O2^xiii—O3—O2^v	96.221 (13)
O2^v—O1—O3^ix	116.23 (2)	O2ⁱⁱ—O3—O2^v	126.20 (2)
O2^vi—O1—O3^ix	63.547 (19)	O2^xiv—O3—O2^v	86.707 (15)
O3^vii—O1—O3^ix	93.827 (18)	O2ⁱⁱⁱ—O3—O2^v	121.723 (19)
O2^viii—O1—O3^ix	58.151 (16)	O1ⁱ—O3—O2^v	68.398 (18)
S—O1—O2^x	124.32 (3)	O1^vii—O3—O2^v	59.707 (17)
Mg^vi—O1—O2^x	95.485 (18)	O1^xiii—O3—O2^v	54.601 (13)
O2—O1—O2^x	159.76 (2)	O1ⁱⁱ—O3—O2^v	99.91 (2)
O1^v—O1—O2^x	100.06 (2)	Mg—O3—O2	42.054 (13)
O2^v—O1—O2^x	106.09 (2)	Mg^v—O3—O2	82.56 (2)
O2^vi—O1—O2^x	76.856 (18)	O2^xiii—O3—O2	126.20 (2)
O3^vii—O1—O2^x	51.431 (14)	O2ⁱⁱ—O3—O2	96.221 (13)
O2^viii—O1—O2^x	110.01 (2)	O2^xiv—O3—O2	121.723 (19)
O3^ix—O1—O2^x	137.453 (19)	O2ⁱⁱⁱ—O3—O2	86.707 (15)
S—O1—O2^vii	111.52 (3)	O1ⁱ—O3—O2	59.707 (16)
Mg^vi—O1—O2^vii	76.748 (18)	O1^vii—O3—O2	68.397 (18)
O2—O1—O2^vii	109.29 (2)	O1^xiii—O3—O2	99.91 (2)
O1^v—O1—O2^vii	137.80 (2)	O1ⁱⁱ—O3—O2	54.602 (13)
O2^v—O1—O2^vii	79.535 (18)	O2^v—O3—O2	46.751 (19)
O2^vi—O1—O2^vii	115.59 (2)	Mg—O3—H	104.9 (10)
O3^vii—O1—O2^vii	57.519 (17)	Mg^v—O3—H	109.2 (10)
O2^viii—O1—O2^vii	44.376 (17)	O2^xiii—O3—H	118.8 (10)
O3^ix—O1—O2^vii	102.370 (18)	O2ⁱⁱ—O3—H	17.8 (10)
O2^x—O1—O2^vii	80.400 (14)	O2^xiv—O3—H	74.0 (10)
S—O1—O3^xi	104.22 (2)	O2ⁱⁱⁱ—O3—H	87.7 (10)
Mg^vi—O1—O3^xi	96.836 (17)	O1ⁱ—O3—H	143.2 (10)
O2—O1—O3^xi	119.40 (2)	O1^vii—O3—H	77.7 (9)
O1^v—O1—O3^xi	69.247 (9)	O1^xiii—O3—H	133.1 (10)
O2^v—O1—O3^xi	118.58 (2)	O1ⁱⁱ—O3—H	65.9 (10)
O2^vi—O1—O3^xi	51.344 (15)	O2^v—O3—H	137.0 (9)
O3^vii—O1—O3^xi	81.949 (15)	O2—O3—H	113.8 (10)
O2^viii—O1—O3^xi	138.117 (17)	Mg—O3—H^v	109.2 (10)
O3^ix—O1—O3^xi	107.284 (18)	Mg^v—O3—H^v	104.9 (10)
O2^x—O1—O3^xi	51.361 (12)	O2^xiii—O3—H^v	17.8 (10)
O2^vii—O1—O3^xi	130.852 (15)	O2ⁱⁱ—O3—H^v	118.8 (10)
S—O2—Mg	133.44 (3)	O2^xiv—O3—H^v	87.7 (10)
S—O2—O1	35.413 (16)	O2ⁱⁱⁱ—O3—H^v	74.0 (10)
Mg—O2—O1	161.95 (2)	O1ⁱ—O3—H^v	77.7 (10)
S—O2—O2^v	35.547 (18)	O1^vii—O3—H^v	143.2 (10)
Mg—O2—O2^v	103.091 (17)	O1^xiii—O3—H^v	65.9 (10)
O1—O2—O2^v	60.413 (18)	O1ⁱⁱ—O3—H^v	133.1 (10)
S—O2—O1^v	34.569 (15)	O2^v—O3—H^v	113.8 (10)
Mg—O2—O1^v	120.20 (2)	O2—O3—H^v	137.0 (10)
O1—O2—O1^v	59.78 (2)	H—O3—H^v	103.6 (19)
O2^v—O2—O1^v	59.374 (18)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱ	0.817 (13)	1.963 (13)	2.7246 (6)	154.9 (13)

Symmetry code: (ii) −x+1/2, y+1/2, −z+1/2.

(MgSO4H2O_N2_193K) top

Crystal data top

Fe₀H₂MgO₅S	V = 354.60 (9) Å³
M_r = 138.39	Z = 4
Monoclinic, C2/c	F(000) = 280
a = 6.8815 (10) Å	D_x = 2.592 Mg m⁻³
b = 7.6534 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.6172 (10) Å	µ = 0.97 mm⁻¹
β = 117.884 (10)°	T = 193 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.020
T_min = 0.686, T_max = 0.748	θ_max = 39.9°, θ_min = 4.2°
9924 measured reflections	h = −12→12
1098 independent reflections	k = −13→13
1047 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.016	w = 1/[σ²(F_o²) + (0.020P)² + 0.180P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.045	(Δ/σ)_max < 0.001
S = 1.20	Δρ_max = 0.49 e Å⁻³
1098 reflections	Δρ_min = −0.37 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.004 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Mg	0.000000	0.500000	0.000000	0.00566 (6)
S	0.000000	0.15635 (2)	0.250000	0.00461 (5)
O1	0.17541 (7)	0.04664 (6)	0.39602 (7)	0.00910 (8)
O2	0.09440 (7)	0.26900 (6)	0.15044 (7)	0.00824 (7)
O3	0.000000	0.63431 (8)	0.250000	0.00757 (9)
H	0.104 (2)	0.7003 (18)	0.291 (2)	0.022 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mg	0.00494 (11)	0.00595 (11)	0.00571 (11)	−0.00034 (8)	0.00217 (9)	0.00024 (8)
S	0.00351 (7)	0.00455 (7)	0.00540 (7)	0.000	0.00177 (5)	0.000
O1	0.00578 (15)	0.01021 (16)	0.01016 (16)	0.00271 (12)	0.00276 (13)	0.00436 (13)
O2	0.00810 (16)	0.00758 (15)	0.01082 (16)	0.00065 (12)	0.00592 (13)	0.00323 (12)
O3	0.0070 (2)	0.0083 (2)	0.0075 (2)	0.000	0.00343 (17)	0.000

Geometric parameters (Å, º) top

Mg—O1ⁱ	2.0222 (5)	O1—O2	2.3939 (6)
Mg—O1ⁱⁱ	2.0222 (5)	O1—O1^v	2.3986 (10)
Mg—O2ⁱⁱⁱ	2.0407 (5)	O1—O2^v	2.4195 (7)
Mg—O2	2.0407 (5)	O1—O2^vi	2.7702 (7)
Mg—O3	2.1640 (4)	O1—O3^vii	2.9230 (7)
Mg—O3ⁱⁱⁱ	2.1640 (4)	O1—O2^viii	2.9721 (8)
Mg—O2ⁱⁱ	3.4882 (6)	O1—O3^ix	3.0001 (6)
Mg—O2ⁱ	3.4882 (6)	O1—O2^x	3.3035 (7)
Mg—O2^iv	3.5007 (6)	O1—O2^vii	3.3640 (8)
Mg—O2^v	3.5007 (6)	O1—O3^xi	3.3759 (9)
Mg—O1^iv	3.8753 (6)	O2—O2^v	2.4148 (9)
Mg—O1^v	3.8753 (6)	O2—O3^ix	2.7292 (6)
S—O1^v	1.4640 (5)	O2—O3ⁱⁱⁱ	2.9018 (6)
S—O1	1.4640 (5)	O2—O3	3.0454 (8)
S—O2^v	1.4837 (5)	O3—H	0.807 (14)
S—O2	1.4837 (5)	O3—H^v	0.807 (14)

O1ⁱ—Mg—O1ⁱⁱ	180.0	S—O2—O3^ix	105.89 (2)
O1ⁱ—Mg—O2ⁱⁱⁱ	85.97 (2)	Mg—O2—O3^ix	119.93 (2)
O1ⁱⁱ—Mg—O2ⁱⁱⁱ	94.03 (2)	O1—O2—O3^ix	71.349 (19)
O1ⁱ—Mg—O2	94.03 (2)	O2^v—O2—O3^ix	127.31 (3)
O1ⁱⁱ—Mg—O2	85.97 (2)	O1^v—O2—O3^ix	112.96 (3)
O2ⁱⁱⁱ—Mg—O2	180.0	S—O2—O1ⁱⁱ	157.56 (3)
O1ⁱ—Mg—O3	88.505 (16)	Mg—O2—O1ⁱⁱ	46.734 (16)
O1ⁱⁱ—Mg—O3	91.495 (16)	O1—O2—O1ⁱⁱ	134.99 (2)
O2ⁱⁱⁱ—Mg—O3	87.23 (2)	O2^v—O2—O1ⁱⁱ	126.015 (17)
O2—Mg—O3	92.77 (2)	O1^v—O2—O1ⁱⁱ	165.10 (3)
O1ⁱ—Mg—O3ⁱⁱⁱ	91.495 (16)	O3^ix—O2—O1ⁱⁱ	75.74 (2)
O1ⁱⁱ—Mg—O3ⁱⁱⁱ	88.505 (16)	S—O2—O3ⁱⁱⁱ	138.52 (3)
O2ⁱⁱⁱ—Mg—O3ⁱⁱⁱ	92.77 (2)	Mg—O2—O3ⁱⁱⁱ	48.149 (15)
O2—Mg—O3ⁱⁱⁱ	87.23 (2)	O1—O2—O3ⁱⁱⁱ	149.15 (3)
O3—Mg—O3ⁱⁱⁱ	180.0	O2^v—O2—O3ⁱⁱⁱ	137.60 (3)
O1ⁱ—Mg—O2ⁱⁱ	138.255 (16)	O1^v—O2—O3ⁱⁱⁱ	104.26 (2)
O1ⁱⁱ—Mg—O2ⁱⁱ	41.745 (16)	O3^ix—O2—O3ⁱⁱⁱ	94.904 (18)
O2ⁱⁱⁱ—Mg—O2ⁱⁱ	81.272 (13)	O1ⁱⁱ—O2—O3ⁱⁱⁱ	61.990 (17)
O2—Mg—O2ⁱⁱ	98.728 (13)	S—O2—O1ⁱ	94.94 (2)
O3—Mg—O2ⁱⁱ	51.482 (13)	Mg—O2—O1ⁱ	42.743 (13)
O3ⁱⁱⁱ—Mg—O2ⁱⁱ	128.518 (12)	O1—O2—O1ⁱ	130.34 (3)
O1ⁱ—Mg—O2ⁱ	41.745 (16)	O2^v—O2—O1ⁱ	76.51 (2)
O1ⁱⁱ—Mg—O2ⁱ	138.255 (16)	O1^v—O2—O1ⁱ	78.14 (2)
O2ⁱⁱⁱ—Mg—O2ⁱ	98.728 (13)	O3^ix—O2—O1ⁱ	156.16 (2)
O2—Mg—O2ⁱ	81.272 (13)	O1ⁱⁱ—O2—O1ⁱ	89.48 (2)
O3—Mg—O2ⁱ	128.518 (12)	O3ⁱⁱⁱ—O2—O1ⁱ	61.414 (16)
O3ⁱⁱⁱ—Mg—O2ⁱ	51.482 (12)	S—O2—O3	102.17 (2)
O2ⁱⁱ—Mg—O2ⁱ	180.0	Mg—O2—O3	45.215 (12)
O1ⁱ—Mg—O2^iv	110.802 (18)	O1—O2—O3	117.19 (2)
O1ⁱⁱ—Mg—O2^iv	69.198 (19)	O2^v—O2—O3	66.642 (10)
O2ⁱⁱⁱ—Mg—O2^iv	42.178 (17)	O1^v—O2—O3	116.34 (2)
O2—Mg—O2^iv	137.821 (17)	O3^ix—O2—O3	125.95 (2)
O3—Mg—O2^iv	120.385 (18)	O1ⁱⁱ—O2—O3	61.898 (16)
O3ⁱⁱⁱ—Mg—O2^iv	59.615 (18)	O3ⁱⁱⁱ—O2—O3	93.364 (15)
O2ⁱⁱ—Mg—O2^iv	85.161 (15)	O1ⁱ—O2—O3	58.108 (13)
O2ⁱ—Mg—O2^iv	94.839 (15)	S—O2—O1^xii	96.27 (2)
O1ⁱ—Mg—O2^v	69.198 (19)	Mg—O2—O1^xii	113.63 (2)
O1ⁱⁱ—Mg—O2^v	110.802 (18)	O1—O2—O1^xii	84.090 (17)
O2ⁱⁱⁱ—Mg—O2^v	137.822 (17)	O2^v—O2—O1^xii	131.029 (14)
O2—Mg—O2^v	42.179 (17)	O1^v—O2—O1^xii	74.24 (2)
O3—Mg—O2^v	59.615 (18)	O3^ix—O2—O1^xii	57.012 (16)
O3ⁱⁱⁱ—Mg—O2^v	120.385 (18)	O1ⁱⁱ—O2—O1^xii	102.856 (19)
O2ⁱⁱ—Mg—O2^v	94.839 (15)	O3ⁱⁱⁱ—O2—O1^xii	65.547 (19)
O2ⁱ—Mg—O2^v	85.161 (15)	O1ⁱ—O2—O1^xii	110.06 (2)
O2^iv—Mg—O2^v	180.0	O3—O2—O1^xii	158.686 (18)
O1ⁱ—Mg—O1^iv	118.071 (18)	S—O2—O1^vii	80.05 (2)
O1ⁱⁱ—Mg—O1^iv	61.929 (18)	Mg—O2—O1^vii	94.97 (2)
O2ⁱⁱⁱ—Mg—O1^iv	32.577 (15)	O1—O2—O1^vii	70.73 (2)
O2—Mg—O1^iv	147.423 (15)	O2^v—O2—O1^vii	59.22 (2)
O3—Mg—O1^iv	83.267 (18)	O1^v—O2—O1^vii	113.94 (2)
O3ⁱⁱⁱ—Mg—O1^iv	96.733 (17)	O3^ix—O2—O1^vii	86.783 (18)
O2ⁱⁱ—Mg—O1^iv	54.058 (12)	O1ⁱⁱ—O2—O1^vii	77.685 (16)
O2ⁱ—Mg—O1^iv	125.943 (12)	O3ⁱⁱⁱ—O2—O1^vii	137.64 (2)
O2^iv—Mg—O1^iv	37.443 (10)	O1ⁱ—O2—O1^vii	108.53 (2)
O2^v—Mg—O1^iv	142.557 (10)	O3—O2—O1^vii	53.988 (12)
O1ⁱ—Mg—O1^v	61.929 (18)	O1^xii—O2—O1^vii	141.406 (17)
O1ⁱⁱ—Mg—O1^v	118.071 (18)	Mg—O3—Mg^v	123.28 (3)
O2ⁱⁱⁱ—Mg—O1^v	147.423 (15)	Mg—O3—O2ⁱⁱ	90.174 (13)
O2—Mg—O1^v	32.577 (15)	Mg^v—O3—O2ⁱⁱ	110.842 (14)
O3—Mg—O1^v	96.733 (17)	Mg—O3—O2^xiii	110.843 (14)
O3ⁱⁱⁱ—Mg—O1^v	83.267 (17)	Mg^v—O3—O2^xiii	90.174 (13)
O2ⁱⁱ—Mg—O1^v	125.942 (12)	O2ⁱⁱ—O3—O2^xiii	135.61 (3)
O2ⁱ—Mg—O1^v	54.057 (12)	Mg—O3—O2^xiv	162.56 (2)
O2^iv—Mg—O1^v	142.557 (10)	Mg^v—O3—O2^xiv	44.622 (11)
O2^v—Mg—O1^v	37.443 (10)	O2ⁱⁱ—O3—O2^xiv	85.096 (18)
O1^iv—Mg—O1^v	180.0	O2^xiii—O3—O2^xiv	83.848 (17)
O1^v—S—O1	110.01 (4)	Mg—O3—O2ⁱⁱⁱ	44.622 (11)
O1^v—S—O2^v	108.61 (3)	Mg^v—O3—O2ⁱⁱⁱ	162.56 (2)
O1—S—O2^v	110.33 (3)	O2ⁱⁱ—O3—O2ⁱⁱⁱ	83.848 (17)
O1^v—S—O2	110.33 (3)	O2^xiii—O3—O2ⁱⁱⁱ	85.096 (18)
O1—S—O2	108.61 (3)	O2^xiv—O3—O2ⁱⁱⁱ	150.45 (3)
O2^v—S—O2	108.94 (4)	Mg—O3—O1ⁱ	43.756 (13)
S—O1—Mg^vi	140.00 (3)	Mg^v—O3—O1ⁱ	105.80 (2)
S—O1—O2	35.970 (17)	O2ⁱⁱ—O3—O1ⁱ	132.554 (15)
Mg^vi—O1—O2	104.03 (2)	O2^xiii—O3—O1ⁱ	71.436 (17)
S—O1—O1^v	35.00 (2)	O2^xiv—O3—O1ⁱ	142.120 (16)
Mg^vi—O1—O1^v	144.24 (3)	O2ⁱⁱⁱ—O3—O1ⁱ	56.794 (16)
O2—O1—O1^v	60.64 (2)	Mg—O3—O1^vii	105.80 (2)
S—O1—O2^v	35.099 (16)	Mg^v—O3—O1^vii	43.756 (13)
Mg^vi—O1—O2^v	144.38 (3)	O2ⁱⁱ—O3—O1^vii	71.436 (17)
O2—O1—O2^v	60.22 (2)	O2^xiii—O3—O1^vii	132.554 (15)
O1^v—O1—O2^v	59.582 (19)	O2^xiv—O3—O1^vii	56.794 (16)
S—O1—O2^vi	131.33 (3)	O2ⁱⁱⁱ—O3—O1^vii	142.120 (16)
Mg^vi—O1—O2^vi	47.294 (14)	O1ⁱ—O3—O1^vii	123.44 (3)
O2—O1—O2^vi	112.55 (2)	Mg—O3—O1^xiii	121.77 (2)
O1^v—O1—O2^vi	105.61 (2)	Mg^v—O3—O1^xiii	42.362 (11)
O2^v—O1—O2^vi	165.10 (3)	O2ⁱⁱ—O3—O1^xiii	145.434 (16)
S—O1—O3^vii	167.26 (3)	O2^xiii—O3—O1^xiii	49.117 (14)
Mg^vi—O1—O3^vii	47.739 (12)	O2^xiv—O3—O1^xiii	60.448 (15)
O2—O1—O3^vii	148.85 (2)	O2ⁱⁱⁱ—O3—O1^xiii	127.393 (15)
O1^v—O1—O3^vii	149.200 (18)	O1ⁱ—O3—O1^xiii	81.708 (17)
O2^v—O1—O3^vii	132.16 (2)	O1^vii—O3—O1^xiii	86.118 (19)
O2^vi—O1—O3^vii	61.217 (17)	Mg—O3—O1ⁱⁱ	42.362 (11)
S—O1—O2^viii	115.27 (3)	Mg^v—O3—O1ⁱⁱ	121.77 (2)
Mg^vi—O1—O2^viii	43.229 (15)	O2ⁱⁱ—O3—O1ⁱⁱ	49.117 (14)
O2—O1—O2^viii	88.419 (19)	O2^xiii—O3—O1ⁱⁱ	145.434 (15)
O1^v—O1—O2^viii	148.586 (18)	O2^xiv—O3—O1ⁱⁱ	127.393 (15)
O2^v—O1—O2^viii	101.86 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	60.448 (15)
O2^vi—O1—O2^viii	90.52 (2)	O1ⁱ—O3—O1ⁱⁱ	86.118 (19)
O3^vii—O1—O2^viii	62.202 (19)	O1^vii—O3—O1ⁱⁱ	81.708 (17)
S—O1—O3^ix	94.72 (2)	O1^xiii—O3—O1ⁱⁱ	154.15 (3)
Mg^vi—O1—O3^ix	46.143 (13)	Mg—O3—O2^v	82.58 (2)
O2—O1—O3^ix	59.534 (18)	Mg^v—O3—O2^v	42.014 (13)
O1^v—O1—O3^ix	104.90 (3)	O2ⁱⁱ—O3—O2^v	125.95 (2)
O2^v—O1—O3^ix	116.23 (2)	O2^xiii—O3—O2^v	96.110 (13)
O2^vi—O1—O3^ix	63.564 (19)	O2^xiv—O3—O2^v	86.636 (15)
O3^vii—O1—O3^ix	93.882 (19)	O2ⁱⁱⁱ—O3—O2^v	121.80 (2)
O2^viii—O1—O3^ix	58.138 (16)	O1ⁱ—O3—O2^v	68.579 (19)
S—O1—O2^x	124.04 (3)	O1^vii—O3—O2^v	59.690 (17)
Mg^vi—O1—O2^x	95.721 (19)	O1^xiii—O3—O2^v	54.539 (14)
O2—O1—O2^x	159.51 (3)	O1ⁱⁱ—O3—O2^v	99.76 (2)
O1^v—O1—O2^x	99.86 (2)	Mg—O3—O2	42.013 (13)
O2^v—O1—O2^x	105.76 (2)	Mg^v—O3—O2	82.58 (2)
O2^vi—O1—O2^x	77.145 (19)	O2ⁱⁱ—O3—O2	96.110 (13)
O3^vii—O1—O2^x	51.552 (15)	O2^xiii—O3—O2	125.95 (2)
O2^viii—O1—O2^x	110.06 (2)	O2^xiv—O3—O2	121.80 (2)
O3^ix—O1—O2^x	137.75 (2)	O2ⁱⁱⁱ—O3—O2	86.636 (15)
S—O1—O2^vii	111.38 (3)	O1ⁱ—O3—O2	59.690 (17)
Mg^vi—O1—O2^vii	76.611 (19)	O1^vii—O3—O2	68.579 (19)
O2—O1—O2^vii	109.27 (2)	O1^xiii—O3—O2	99.76 (2)
O1^v—O1—O2^vii	137.62 (2)	O1ⁱⁱ—O3—O2	54.539 (14)
O2^v—O1—O2^vii	79.384 (19)	O2^v—O3—O2	46.72 (2)
O2^vi—O1—O2^vii	115.48 (2)	Mg—O3—H	105.8 (10)
O3^vii—O1—O2^vii	57.433 (18)	Mg^v—O3—H	108.8 (10)
O2^viii—O1—O2^vii	44.270 (18)	O2ⁱⁱ—O3—H	18.8 (10)
O3^ix—O1—O2^vii	102.256 (19)	O2^xiii—O3—H	118.3 (10)
O2^x—O1—O2^vii	80.320 (15)	O2^xiv—O3—H	73.3 (10)
S—O1—O3^xi	104.19 (2)	O2ⁱⁱⁱ—O3—H	88.2 (10)
Mg^vi—O1—O3^xi	97.082 (18)	O1ⁱ—O3—H	143.8 (10)
O2—O1—O3^xi	119.37 (2)	O1^vii—O3—H	77.6 (10)
O1^v—O1—O3^xi	69.191 (9)	O1^xiii—O3—H	132.3 (10)
O2^v—O1—O3^xi	118.53 (2)	O1ⁱⁱ—O3—H	66.8 (10)
O2^vi—O1—O3^xi	51.582 (15)	O2^v—O3—H	137.0 (10)
O3^vii—O1—O3^xi	82.084 (16)	O2—O3—H	114.7 (10)
O2^viii—O1—O3^xi	138.327 (17)	Mg—O3—H^v	108.8 (10)
O3^ix—O1—O3^xi	107.482 (19)	Mg^v—O3—H^v	105.8 (10)
O2^x—O1—O3^xi	51.485 (13)	O2ⁱⁱ—O3—H^v	118.3 (10)
O2^vii—O1—O3^xi	130.882 (16)	O2^xiii—O3—H^v	18.8 (10)
S—O2—Mg	133.63 (3)	O2^xiv—O3—H^v	88.2 (10)
S—O2—O1	35.421 (16)	O2ⁱⁱⁱ—O3—H^v	73.3 (10)
Mg—O2—O1	162.05 (3)	O1ⁱ—O3—H^v	77.6 (10)
S—O2—O2^v	35.530 (19)	O1^vii—O3—H^v	143.8 (10)
Mg—O2—O2^v	103.251 (17)	O1^xiii—O3—H^v	66.8 (10)
O1—O2—O2^v	60.416 (19)	O1ⁱⁱ—O3—H^v	132.3 (10)
S—O2—O1^v	34.567 (16)	O2^v—O3—H^v	114.7 (10)
Mg—O2—O1^v	120.41 (2)	O2—O3—H^v	137.0 (10)
O1—O2—O1^v	59.77 (3)	H—O3—H^v	103 (2)
O2^v—O2—O1^v	59.364 (18)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱ	0.807 (14)	1.982 (14)	2.7292 (6)	153.7 (14)

Symmetry code: (ii) −x+1/2, y+1/2, −z+1/2.

(MgSO4H2O_N2_233K) top

Crystal data top

Fe₀H₂MgO₅S	V = 355.20 (9) Å³
M_r = 138.39	Z = 4
Monoclinic, C2/c	F(000) = 280
a = 6.8937 (10) Å	D_x = 2.588 Mg m⁻³
b = 7.6466 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.6275 (10) Å	µ = 0.97 mm⁻¹
β = 117.943 (10)°	T = 233 K

Data collection top

9888 measured reflections	θ_max = 40.0°, θ_min = 4.2°
1100 independent reflections	h = −12→12
1050 reflections with I > 2σ(I)	k = −13→13
R_int = 0.019	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.015	w = 1/[σ²(F_o²) + (0.019P)² + 0.190P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.045	(Δ/σ)_max < 0.001
S = 1.20	Δρ_max = 0.52 e Å⁻³
1100 reflections	Δρ_min = −0.41 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0051 (19)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Mg	0.000000	0.500000	0.000000	0.00652 (6)
S	0.000000	0.15586 (2)	0.250000	0.00530 (5)
O1	0.17551 (7)	0.04607 (6)	0.39547 (7)	0.01054 (8)
O2	0.09346 (7)	0.26857 (6)	0.15003 (7)	0.00955 (8)
O3	0.000000	0.63464 (8)	0.250000	0.00867 (10)
H	0.103 (2)	0.7020 (18)	0.291 (2)	0.024 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mg	0.00574 (11)	0.00680 (11)	0.00652 (11)	−0.00039 (8)	0.00244 (9)	0.00034 (8)
S	0.00400 (7)	0.00518 (7)	0.00623 (7)	0.000	0.00198 (5)	0.000
O1	0.00642 (15)	0.01185 (17)	0.01192 (17)	0.00311 (13)	0.00312 (13)	0.00518 (13)
O2	0.00931 (17)	0.00875 (16)	0.01258 (17)	0.00087 (12)	0.00678 (14)	0.00375 (12)
O3	0.0082 (2)	0.0095 (2)	0.0084 (2)	0.000	0.00396 (18)	0.000

Geometric parameters (Å, º) top

Mg—O1ⁱ	2.0229 (6)	O1—O2	2.3931 (7)
Mg—O1ⁱⁱ	2.0229 (6)	O1—O1^v	2.3974 (10)
Mg—O2ⁱⁱⁱ	2.0409 (5)	O1—O2^v	2.4187 (7)
Mg—O2	2.0409 (5)	O1—O2^vi	2.7709 (7)
Mg—O3	2.1671 (4)	O1—O3^vii	2.9252 (7)
Mg—O3ⁱⁱⁱ	2.1671 (4)	O1—O2^viii	2.9728 (8)
Mg—O2ⁱⁱ	3.4909 (6)	O1—O3^ix	3.0033 (6)
Mg—O2ⁱ	3.4909 (6)	O1—O2^x	3.3027 (7)
Mg—O2^iv	3.5049 (6)	O1—O3^xi	3.3667 (9)
Mg—O2^v	3.5049 (6)	O1—O2^vii	3.3747 (8)
Mg—O1^iv	3.8796 (6)	O2—O2^v	2.4141 (9)
Mg—O1^v	3.8796 (6)	O2—O3^ix	2.7353 (6)
S—O1^v	1.4634 (5)	O2—O3ⁱⁱⁱ	2.9035 (6)
S—O1	1.4634 (5)	O2—O3	3.0483 (8)
S—O2^v	1.4832 (5)	O3—H	0.813 (14)
S—O2	1.4832 (5)	O3—H^v	0.813 (14)

O1ⁱ—Mg—O1ⁱⁱ	180.0	S—O2—O3^ix	105.92 (3)
O1ⁱ—Mg—O2ⁱⁱⁱ	85.97 (2)	Mg—O2—O3^ix	119.60 (2)
O1ⁱⁱ—Mg—O2ⁱⁱⁱ	94.03 (2)	O1—O2—O3^ix	71.340 (19)
O1ⁱ—Mg—O2	94.03 (2)	O2^v—O2—O3^ix	127.18 (3)
O1ⁱⁱ—Mg—O2	85.97 (2)	O1^v—O2—O3^ix	113.15 (3)
O2ⁱⁱⁱ—Mg—O2	180.0	S—O2—O1ⁱⁱ	157.38 (3)
O1ⁱ—Mg—O3	88.488 (17)	Mg—O2—O1ⁱⁱ	46.741 (16)
O1ⁱⁱ—Mg—O3	91.512 (17)	O1—O2—O1ⁱⁱ	134.70 (2)
O2ⁱⁱⁱ—Mg—O3	87.21 (2)	O2^v—O2—O1ⁱⁱ	125.973 (17)
O2—Mg—O3	92.79 (2)	O1^v—O2—O1ⁱⁱ	165.40 (3)
O1ⁱ—Mg—O3ⁱⁱⁱ	91.512 (16)	O3^ix—O2—O1ⁱⁱ	75.38 (2)
O1ⁱⁱ—Mg—O3ⁱⁱⁱ	88.488 (17)	S—O2—O3ⁱⁱⁱ	138.80 (3)
O2ⁱⁱⁱ—Mg—O3ⁱⁱⁱ	92.79 (2)	Mg—O2—O3ⁱⁱⁱ	48.199 (15)
O2—Mg—O3ⁱⁱⁱ	87.21 (2)	O1—O2—O3ⁱⁱⁱ	149.09 (3)
O3—Mg—O3ⁱⁱⁱ	180.0	O2^v—O2—O3ⁱⁱⁱ	137.95 (3)
O1ⁱ—Mg—O2ⁱⁱ	138.340 (16)	O1^v—O2—O3ⁱⁱⁱ	104.53 (2)
O1ⁱⁱ—Mg—O2ⁱⁱ	41.660 (16)	O3^ix—O2—O3ⁱⁱⁱ	94.715 (18)
O2ⁱⁱⁱ—Mg—O2ⁱⁱ	81.260 (13)	O1ⁱⁱ—O2—O3ⁱⁱⁱ	62.011 (17)
O2—Mg—O2ⁱⁱ	98.740 (13)	S—O2—O1ⁱ	95.24 (2)
O3—Mg—O2ⁱⁱ	51.587 (12)	Mg—O2—O1ⁱ	42.749 (13)
O3ⁱⁱⁱ—Mg—O2ⁱⁱ	128.413 (12)	O1—O2—O1ⁱ	130.64 (3)
O1ⁱ—Mg—O2ⁱ	41.660 (16)	O2^v—O2—O1ⁱ	76.81 (2)
O1ⁱⁱ—Mg—O2ⁱ	138.340 (16)	O1^v—O2—O1ⁱ	78.37 (2)
O2ⁱⁱⁱ—Mg—O2ⁱ	98.740 (13)	O3^ix—O2—O1ⁱ	155.98 (2)
O2—Mg—O2ⁱ	81.261 (13)	O1ⁱⁱ—O2—O1ⁱ	89.49 (2)
O3—Mg—O2ⁱ	128.413 (12)	O3ⁱⁱⁱ—O2—O1ⁱ	61.458 (16)
O3ⁱⁱⁱ—Mg—O2ⁱ	51.587 (12)	S—O2—O3	102.20 (2)
O2ⁱⁱ—Mg—O2ⁱ	180.0	Mg—O2—O3	45.239 (12)
O1ⁱ—Mg—O2^iv	110.592 (19)	O1—O2—O3	117.22 (2)
O1ⁱⁱ—Mg—O2^iv	69.408 (19)	O2^v—O2—O3	66.674 (10)
O2ⁱⁱⁱ—Mg—O2^iv	42.059 (17)	O1^v—O2—O3	116.37 (2)
O2—Mg—O2^iv	137.941 (17)	O3^ix—O2—O3	125.67 (2)
O3—Mg—O2^iv	120.404 (18)	O1ⁱⁱ—O2—O3	61.925 (16)
O3ⁱⁱⁱ—Mg—O2^iv	59.596 (19)	O3ⁱⁱⁱ—O2—O3	93.438 (16)
O2ⁱⁱ—Mg—O2^iv	85.246 (15)	O1ⁱ—O2—O3	58.117 (13)
O2ⁱ—Mg—O2^iv	94.754 (15)	S—O2—O1^xii	96.56 (2)
O1ⁱ—Mg—O2^v	69.408 (19)	Mg—O2—O1^xii	113.46 (2)
O1ⁱⁱ—Mg—O2^v	110.592 (19)	O1—O2—O1^xii	84.214 (17)
O2ⁱⁱⁱ—Mg—O2^v	137.941 (17)	O2^v—O2—O1^xii	131.342 (14)
O2—Mg—O2^v	42.059 (17)	O1^v—O2—O1^xii	74.59 (2)
O3—Mg—O2^v	59.596 (18)	O3^ix—O2—O1^xii	57.028 (16)
O3ⁱⁱⁱ—Mg—O2^v	120.404 (19)	O1ⁱⁱ—O2—O1^xii	102.56 (2)
O2ⁱⁱ—Mg—O2^v	94.754 (15)	O3ⁱⁱⁱ—O2—O1^xii	65.334 (19)
O2ⁱ—Mg—O2^v	85.246 (16)	O1ⁱ—O2—O1^xii	110.11 (2)
O2^iv—Mg—O2^v	180.0	O3—O2—O1^xii	158.511 (18)
O1ⁱ—Mg—O1^iv	117.942 (19)	S—O2—O1^vii	79.95 (2)
O1ⁱⁱ—Mg—O1^iv	62.058 (19)	Mg—O2—O1^vii	94.87 (2)
O2ⁱⁱⁱ—Mg—O1^iv	32.427 (15)	O1—O2—O1^vii	70.74 (2)
O2—Mg—O1^iv	147.572 (15)	O2^v—O2—O1^vii	59.05 (2)
O3—Mg—O1^iv	83.361 (18)	O1^v—O2—O1^vii	113.82 (2)
O3ⁱⁱⁱ—Mg—O1^iv	96.640 (18)	O3^ix—O2—O1^vii	86.687 (19)
O2ⁱⁱ—Mg—O1^iv	54.188 (12)	O1ⁱⁱ—O2—O1^vii	77.571 (16)
O2ⁱ—Mg—O1^iv	125.811 (12)	O3ⁱⁱⁱ—O2—O1^vii	137.56 (2)
O2^iv—Mg—O1^iv	37.384 (10)	O1ⁱ—O2—O1^vii	108.49 (2)
O2^v—Mg—O1^iv	142.616 (10)	O3—O2—O1^vii	53.894 (12)
O1ⁱ—Mg—O1^v	62.058 (19)	O1^xii—O2—O1^vii	141.396 (18)
O1ⁱⁱ—Mg—O1^v	117.942 (19)	Mg—O3—Mg^v	123.27 (3)
O2ⁱⁱⁱ—Mg—O1^v	147.573 (15)	Mg—O3—O2ⁱⁱ	90.040 (13)
O2—Mg—O1^v	32.428 (16)	Mg^v—O3—O2ⁱⁱ	110.797 (14)
O3—Mg—O1^v	96.639 (18)	Mg—O3—O2^xiii	110.797 (14)
O3ⁱⁱⁱ—Mg—O1^v	83.360 (18)	Mg^v—O3—O2^xiii	90.040 (13)
O2ⁱⁱ—Mg—O1^v	125.812 (12)	O2ⁱⁱ—O3—O2^xiii	136.02 (3)
O2ⁱ—Mg—O1^v	54.189 (12)	Mg—O3—O2^xiv	162.61 (2)
O2^iv—Mg—O1^v	142.616 (10)	Mg^v—O3—O2^xiv	44.594 (12)
O2^v—Mg—O1^v	37.384 (10)	O2ⁱⁱ—O3—O2^xiv	85.285 (18)
O1^iv—Mg—O1^v	180.0	O2^xiii—O3—O2^xiv	83.762 (17)
O1^v—S—O1	109.99 (4)	Mg—O3—O2ⁱⁱⁱ	44.594 (12)
O1^v—S—O2^v	108.61 (3)	Mg^v—O3—O2ⁱⁱⁱ	162.61 (2)
O1—S—O2^v	110.34 (3)	O2ⁱⁱ—O3—O2ⁱⁱⁱ	83.762 (17)
O1^v—S—O2	110.34 (3)	O2^xiii—O3—O2ⁱⁱⁱ	85.284 (18)
O1—S—O2	108.61 (3)	O2^xiv—O3—O2ⁱⁱⁱ	150.46 (3)
O2^v—S—O2	108.94 (4)	Mg—O3—O1ⁱ	43.733 (13)
S—O1—Mg^vi	140.12 (3)	Mg^v—O3—O1ⁱ	105.89 (2)
S—O1—O2	35.970 (17)	O2ⁱⁱ—O3—O1ⁱ	132.403 (15)
Mg^vi—O1—O2	104.15 (2)	O2^xiii—O3—O1ⁱ	71.300 (17)
S—O1—O1^v	35.00 (2)	O2^xiv—O3—O1ⁱ	142.081 (17)
Mg^vi—O1—O1^v	144.58 (3)	O2ⁱⁱⁱ—O3—O1ⁱ	56.766 (16)
O2—O1—O1^v	60.65 (2)	Mg—O3—O1^vii	105.89 (2)
S—O1—O2^v	35.099 (17)	Mg^v—O3—O1^vii	43.733 (13)
Mg^vi—O1—O2^v	144.18 (3)	O2ⁱⁱ—O3—O1^vii	71.300 (17)
O2—O1—O2^v	60.22 (2)	O2^xiii—O3—O1^vii	132.403 (15)
O1^v—O1—O2^v	59.587 (19)	O2^xiv—O3—O1^vii	56.766 (16)
S—O1—O2^vi	131.59 (3)	O2ⁱⁱⁱ—O3—O1^vii	142.081 (17)
Mg^vi—O1—O2^vi	47.286 (14)	O1ⁱ—O3—O1^vii	123.62 (3)
O2—O1—O2^vi	112.67 (2)	Mg—O3—O1^xiii	121.67 (2)
O1^v—O1—O2^vi	105.91 (2)	Mg^v—O3—O1^xiii	42.325 (12)
O2^v—O1—O2^vi	165.40 (3)	O2ⁱⁱ—O3—O1^xiii	145.555 (16)
S—O1—O3^vii	166.98 (3)	O2^xiii—O3—O1^xiii	49.019 (15)
Mg^vi—O1—O3^vii	47.780 (12)	O2^xiv—O3—O1^xiii	60.406 (16)
O2—O1—O3^vii	148.99 (2)	O2ⁱⁱⁱ—O3—O1^xiii	127.504 (15)
O1^v—O1—O3^vii	149.163 (18)	O1ⁱ—O3—O1^xiii	81.704 (17)
O2^v—O1—O3^vii	131.89 (2)	O1^vii—O3—O1^xiii	86.057 (19)
O2^vi—O1—O3^vii	61.222 (17)	Mg—O3—O1ⁱⁱ	42.325 (11)
S—O1—O2^viii	115.19 (3)	Mg^v—O3—O1ⁱⁱ	121.67 (2)
Mg^vi—O1—O2^viii	43.223 (15)	O2ⁱⁱ—O3—O1ⁱⁱ	49.019 (15)
O2—O1—O2^viii	88.48 (2)	O2^xiii—O3—O1ⁱⁱ	145.554 (16)
O1^v—O1—O2^viii	148.599 (18)	O2^xiv—O3—O1ⁱⁱ	127.504 (15)
O2^v—O1—O2^viii	101.63 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	60.406 (15)
O2^vi—O1—O2^viii	90.51 (2)	O1ⁱ—O3—O1ⁱⁱ	86.057 (18)
O3^vii—O1—O2^viii	62.236 (19)	O1^vii—O3—O1ⁱⁱ	81.704 (17)
S—O1—O3^ix	94.87 (2)	O1^xiii—O3—O1ⁱⁱ	153.94 (3)
Mg^vi—O1—O3^ix	46.163 (14)	Mg—O3—O2	41.969 (14)
O2—O1—O3^ix	59.641 (19)	Mg^v—O3—O2	82.59 (2)
O1^v—O1—O3^ix	105.16 (3)	O2ⁱⁱ—O3—O2	95.998 (14)
O2^v—O1—O3^ix	116.23 (2)	O2^xiii—O3—O2	125.67 (2)
O2^vi—O1—O3^ix	63.58 (2)	O2^xiv—O3—O2	121.88 (2)
O3^vii—O1—O3^ix	93.943 (19)	O2ⁱⁱⁱ—O3—O2	86.562 (16)
O2^viii—O1—O3^ix	58.135 (16)	O1ⁱ—O3—O2	59.648 (18)
S—O1—O2^x	123.72 (3)	O1^vii—O3—O2	68.761 (19)
Mg^vi—O1—O2^x	95.958 (19)	O1^xiii—O3—O2	99.59 (2)
O2—O1—O2^x	159.23 (3)	O1ⁱⁱ—O3—O2	54.493 (14)
O1^v—O1—O2^x	99.64 (2)	Mg—O3—O2^v	82.59 (2)
O2^v—O1—O2^x	105.42 (2)	Mg^v—O3—O2^v	41.969 (14)
O2^vi—O1—O2^x	77.444 (19)	O2ⁱⁱ—O3—O2^v	125.67 (2)
O3^vii—O1—O2^x	51.672 (15)	O2^xiii—O3—O2^v	95.998 (13)
O2^viii—O1—O2^x	110.12 (2)	O2^xiv—O3—O2^v	86.562 (16)
O3^ix—O1—O2^x	138.06 (2)	O2ⁱⁱⁱ—O3—O2^v	121.88 (2)
S—O1—O3^xi	104.15 (3)	O1ⁱ—O3—O2^v	68.762 (19)
Mg^vi—O1—O3^xi	97.320 (18)	O1^vii—O3—O2^v	59.647 (18)
O2—O1—O3^xi	119.33 (2)	O1^xiii—O3—O2^v	54.493 (14)
O1^v—O1—O3^xi	69.142 (9)	O1ⁱⁱ—O3—O2^v	99.59 (2)
O2^v—O1—O3^xi	118.49 (2)	O2—O3—O2^v	46.65 (2)
O2^vi—O1—O3^xi	51.829 (15)	Mg—O3—H	106.2 (10)
O3^vii—O1—O3^xi	82.200 (16)	Mg^v—O3—H	108.8 (10)
O2^viii—O1—O3^xi	138.542 (18)	O2ⁱⁱ—O3—H	19.6 (10)
O3^ix—O1—O3^xi	107.688 (19)	O2^xiii—O3—H	117.9 (10)
O2^x—O1—O3^xi	51.605 (13)	O2^xiv—O3—H	73.2 (10)
S—O1—O2^vii	111.25 (3)	O2ⁱⁱⁱ—O3—H	88.1 (10)
Mg^vi—O1—O2^vii	76.459 (19)	O1ⁱ—O3—H	143.9 (10)
O2—O1—O2^vii	109.26 (2)	O1^vii—O3—H	77.9 (10)
O1^v—O1—O2^vii	137.45 (3)	O1^xiii—O3—H	132.0 (10)
O2^v—O1—O2^vii	79.224 (19)	O1ⁱⁱ—O3—H	67.4 (10)
O2^vi—O1—O2^vii	115.34 (2)	O2—O3—H	115.4 (10)
O3^vii—O1—O2^vii	57.346 (18)	O2^v—O3—H	137.3 (10)
O2^viii—O1—O2^vii	44.143 (18)	Mg—O3—H^v	108.8 (10)
O3^ix—O1—O2^vii	102.130 (19)	Mg^v—O3—H^v	106.2 (10)
O2^x—O1—O2^vii	80.237 (15)	O2ⁱⁱ—O3—H^v	117.9 (10)
O3^xi—O1—O2^vii	130.901 (16)	O2^xiii—O3—H^v	19.6 (10)
S—O2—Mg	133.87 (3)	O2^xiv—O3—H^v	88.1 (10)
S—O2—O1	35.419 (16)	O2ⁱⁱⁱ—O3—H^v	73.2 (10)
Mg—O2—O1	162.15 (3)	O1ⁱ—O3—H^v	77.9 (10)
S—O2—O2^v	35.528 (19)	O1^vii—O3—H^v	143.9 (10)
Mg—O2—O2^v	103.444 (17)	O1^xiii—O3—H^v	67.4 (10)
O1—O2—O2^v	60.414 (19)	O1ⁱⁱ—O3—H^v	132.0 (10)
S—O2—O1^v	34.564 (17)	O2—O3—H^v	137.3 (10)
Mg—O2—O1^v	120.67 (3)	O2^v—O3—H^v	115.4 (10)
O1—O2—O1^v	59.76 (3)	H—O3—H^v	101 (2)
O2^v—O2—O1^v	59.362 (19)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱ	0.813 (14)	1.988 (14)	2.7353 (6)	152.5 (14)

Symmetry code: (ii) −x+1/2, y+1/2, −z+1/2.

(MgSO4H2O_N2_273K) top

Crystal data top

Fe₀H₂MgO₅S	V = 355.57 (9) Å³
M_r = 138.39	Z = 4
Monoclinic, C2/c	F(000) = 280
a = 6.907 (1) Å	D_x = 2.585 Mg m⁻³
b = 7.6356 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.6373 (10) Å	µ = 0.97 mm⁻¹
β = 118.021 (10)°	T = 273 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.019
T_min = 0.691, T_max = 0.748	θ_max = 40.0°, θ_min = 4.2°
9929 measured reflections	h = −12→12
1101 independent reflections	k = −13→13
1058 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.016	w = 1/[σ²(F_o²) + (0.020P)² + 0.170P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.046	(Δ/σ)_max < 0.001
S = 1.21	Δρ_max = 0.52 e Å⁻³
1101 reflections	Δρ_min = −0.37 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.005 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Mg	0.000000	0.500000	0.000000	0.00746 (6)
S	0.000000	0.15529 (2)	0.250000	0.00604 (5)
O1	0.17569 (7)	0.04536 (7)	0.39486 (7)	0.01209 (8)
O2	0.09235 (8)	0.26806 (6)	0.14957 (7)	0.01101 (8)
O3	0.000000	0.63497 (9)	0.250000	0.00991 (10)
H	0.104 (2)	0.7024 (18)	0.293 (2)	0.025 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mg	0.00655 (12)	0.00777 (12)	0.00747 (11)	−0.00039 (8)	0.00280 (9)	0.00049 (8)
S	0.00453 (7)	0.00592 (7)	0.00710 (7)	0.000	0.00226 (5)	0.000
O1	0.00720 (16)	0.01384 (18)	0.01366 (17)	0.00361 (13)	0.00358 (13)	0.00604 (14)
O2	0.01084 (17)	0.01001 (16)	0.01447 (17)	0.00112 (12)	0.00785 (14)	0.00436 (13)
O3	0.0095 (2)	0.0108 (2)	0.0096 (2)	0.000	0.00462 (18)	0.000

Geometric parameters (Å, º) top

Mg—O1ⁱ	2.0230 (6)	O1—O2	2.3914 (7)
Mg—O1ⁱⁱ	2.0230 (6)	O1—O1^v	2.3959 (10)
Mg—O2ⁱⁱⁱ	2.0405 (5)	O1—O2^v	2.4174 (7)
Mg—O2	2.0405 (5)	O1—O2^vi	2.7706 (7)
Mg—O3ⁱⁱⁱ	2.1697 (4)	O1—O3^vii	2.9260 (7)
Mg—O3	2.1697 (4)	O1—O2^viii	2.9725 (8)
Mg—O2ⁱ	3.4928 (6)	O1—O3^ix	3.0063 (6)
Mg—O2ⁱⁱ	3.4928 (6)	O1—O2^x	3.3007 (7)
Mg—O2^iv	3.5086 (6)	O1—O3^xi	3.3548 (9)
Mg—O2^v	3.5086 (6)	O1—O2^vii	3.3859 (8)
Mg—O1^iv	3.8838 (7)	O2—O2^v	2.4123 (10)
Mg—O1^v	3.8838 (7)	O2—O3^ix	2.7422 (6)
S—O1	1.4628 (5)	O2—O3ⁱⁱⁱ	2.9050 (6)
S—O1^v	1.4628 (5)	O2—O3	3.0502 (8)
S—O2	1.4820 (5)	O3—H	0.816 (14)
S—O2^v	1.4820 (5)	O3—H^v	0.816 (14)

O1ⁱ—Mg—O1ⁱⁱ	180.0	S—O2—O3^ix	105.96 (3)
O1ⁱ—Mg—O2ⁱⁱⁱ	85.97 (2)	Mg—O2—O3^ix	119.21 (2)
O1ⁱⁱ—Mg—O2ⁱⁱⁱ	94.03 (2)	O1—O2—O3^ix	71.32 (2)
O1ⁱ—Mg—O2	94.03 (2)	O2^v—O2—O3^ix	127.04 (3)
O1ⁱⁱ—Mg—O2	85.97 (2)	O1^v—O2—O3^ix	113.36 (3)
O2ⁱⁱⁱ—Mg—O2	179.999 (12)	S—O2—O1ⁱⁱ	157.18 (3)
O1ⁱ—Mg—O3ⁱⁱⁱ	91.556 (17)	Mg—O2—O1ⁱⁱ	46.749 (16)
O1ⁱⁱ—Mg—O3ⁱⁱⁱ	88.444 (18)	O1—O2—O1ⁱⁱ	134.36 (2)
O2ⁱⁱⁱ—Mg—O3ⁱⁱⁱ	92.80 (2)	O2^v—O2—O1ⁱⁱ	125.936 (18)
O2—Mg—O3ⁱⁱⁱ	87.20 (2)	O1^v—O2—O1ⁱⁱ	165.74 (3)
O1ⁱ—Mg—O3	88.444 (17)	O3^ix—O2—O1ⁱⁱ	74.97 (2)
O1ⁱⁱ—Mg—O3	91.556 (17)	S—O2—O3ⁱⁱⁱ	139.14 (3)
O2ⁱⁱⁱ—Mg—O3	87.20 (2)	Mg—O2—O3ⁱⁱⁱ	48.244 (16)
O2—Mg—O3	92.80 (2)	O1—O2—O3ⁱⁱⁱ	149.03 (3)
O3ⁱⁱⁱ—Mg—O3	180.0	O2^v—O2—O3ⁱⁱⁱ	138.35 (3)
O1ⁱ—Mg—O2ⁱ	41.568 (16)	O1^v—O2—O3ⁱⁱⁱ	104.84 (2)
O1ⁱⁱ—Mg—O2ⁱ	138.432 (17)	O3^ix—O2—O3ⁱⁱⁱ	94.482 (19)
O2ⁱⁱⁱ—Mg—O2ⁱ	98.754 (13)	O1ⁱⁱ—O2—O3ⁱⁱⁱ	62.014 (18)
O2—Mg—O2ⁱ	81.246 (13)	S—O2—O1ⁱ	95.59 (3)
O3ⁱⁱⁱ—Mg—O2ⁱ	51.730 (13)	Mg—O2—O1ⁱ	42.755 (13)
O3—Mg—O2ⁱ	128.270 (13)	O1—O2—O1ⁱ	131.01 (3)
O1ⁱ—Mg—O2ⁱⁱ	138.432 (16)	O2^v—O2—O1ⁱ	77.14 (2)
O1ⁱⁱ—Mg—O2ⁱⁱ	41.568 (16)	O1^v—O2—O1ⁱ	78.65 (2)
O2ⁱⁱⁱ—Mg—O2ⁱⁱ	81.246 (13)	O3^ix—O2—O1ⁱ	155.76 (2)
O2—Mg—O2ⁱⁱ	98.754 (13)	O1ⁱⁱ—O2—O1ⁱ	89.50 (2)
O3ⁱⁱⁱ—Mg—O2ⁱⁱ	128.269 (13)	O3ⁱⁱⁱ—O2—O1ⁱ	61.515 (17)
O3—Mg—O2ⁱⁱ	51.731 (13)	S—O2—O3	102.23 (2)
O2ⁱ—Mg—O2ⁱⁱ	180.0	Mg—O2—O3	45.274 (13)
O1ⁱ—Mg—O2^iv	110.36 (2)	O1—O2—O3	117.25 (2)
O1ⁱⁱ—Mg—O2^iv	69.64 (2)	O2^v—O2—O3	66.707 (10)
O2ⁱⁱⁱ—Mg—O2^iv	41.919 (18)	O1^v—O2—O3	116.39 (2)
O2—Mg—O2^iv	138.082 (18)	O3^ix—O2—O3	125.35 (2)
O3ⁱⁱⁱ—Mg—O2^iv	59.558 (19)	O1ⁱⁱ—O2—O3	61.975 (17)
O3—Mg—O2^iv	120.442 (19)	O3ⁱⁱⁱ—O2—O3	93.519 (16)
O2ⁱ—Mg—O2^iv	94.664 (16)	O1ⁱ—O2—O3	58.116 (14)
O2ⁱⁱ—Mg—O2^iv	85.336 (15)	S—O2—O1^xii	96.92 (3)
O1ⁱ—Mg—O2^v	69.64 (2)	Mg—O2—O1^xii	113.24 (2)
O1ⁱⁱ—Mg—O2^v	110.36 (2)	O1—O2—O1^xii	84.359 (17)
O2ⁱⁱⁱ—Mg—O2^v	138.081 (18)	O2^v—O2—O1^xii	131.723 (15)
O2—Mg—O2^v	41.918 (18)	O1^v—O2—O1^xii	75.01 (2)
O3ⁱⁱⁱ—Mg—O2^v	120.442 (19)	O3^ix—O2—O1^xii	57.024 (17)
O3—Mg—O2^v	59.558 (19)	O1ⁱⁱ—O2—O1^xii	102.18 (2)
O2ⁱ—Mg—O2^v	85.336 (16)	O3ⁱⁱⁱ—O2—O1^xii	65.08 (2)
O2ⁱⁱ—Mg—O2^v	94.664 (15)	O1ⁱ—O2—O1^xii	110.19 (2)
O2^iv—Mg—O2^v	180.0	O3—O2—O1^xii	158.295 (19)
O1ⁱ—Mg—O1^iv	117.79 (2)	S—O2—O1^vii	79.84 (2)
O1ⁱⁱ—Mg—O1^iv	62.21 (2)	Mg—O2—O1^vii	94.74 (2)
O2ⁱⁱⁱ—Mg—O1^iv	32.257 (16)	O1—O2—O1^vii	70.77 (2)
O2—Mg—O1^iv	147.744 (16)	O2^v—O2—O1^vii	58.86 (2)
O3ⁱⁱⁱ—Mg—O1^iv	96.513 (18)	O1^v—O2—O1^vii	113.68 (2)
O3—Mg—O1^iv	83.487 (18)	O3^ix—O2—O1^vii	86.591 (19)
O2ⁱ—Mg—O1^iv	125.667 (13)	O1ⁱⁱ—O2—O1^vii	77.444 (16)
O2ⁱⁱ—Mg—O1^iv	54.333 (13)	O3ⁱⁱⁱ—O2—O1^vii	137.44 (2)
O2^iv—Mg—O1^iv	37.315 (10)	O1ⁱ—O2—O1^vii	108.43 (2)
O2^v—Mg—O1^iv	142.685 (10)	O3—O2—O1^vii	53.774 (12)
O1ⁱ—Mg—O1^v	62.21 (2)	O1^xii—O2—O1^vii	141.384 (18)
O1ⁱⁱ—Mg—O1^v	117.79 (2)	Mg—O3—Mg^v	123.28 (3)
O2ⁱⁱⁱ—Mg—O1^v	147.743 (16)	Mg—O3—O2^xiii	110.755 (15)
O2—Mg—O1^v	32.256 (16)	Mg^v—O3—O2^xiii	89.866 (13)
O3ⁱⁱⁱ—Mg—O1^v	83.487 (18)	Mg—O3—O2ⁱⁱ	89.866 (13)
O3—Mg—O1^v	96.513 (18)	Mg^v—O3—O2ⁱⁱ	110.755 (15)
O2ⁱ—Mg—O1^v	54.333 (13)	O2^xiii—O3—O2ⁱⁱ	136.50 (3)
O2ⁱⁱ—Mg—O1^v	125.667 (13)	Mg—O3—O2^xiv	162.69 (2)
O2^iv—Mg—O1^v	142.685 (10)	Mg^v—O3—O2^xiv	44.554 (12)
O2^v—Mg—O1^v	37.315 (10)	O2^xiii—O3—O2^xiv	83.641 (17)
O1^iv—Mg—O1^v	180.0	O2ⁱⁱ—O3—O2^xiv	85.517 (19)
O1—S—O1^v	109.96 (4)	Mg—O3—O2ⁱⁱⁱ	44.554 (12)
O1—S—O2	108.60 (3)	Mg^v—O3—O2ⁱⁱⁱ	162.69 (2)
O1^v—S—O2	110.35 (3)	O2^xiii—O3—O2ⁱⁱⁱ	85.517 (19)
O1—S—O2^v	110.35 (3)	O2ⁱⁱ—O3—O2ⁱⁱⁱ	83.641 (17)
O1^v—S—O2^v	108.60 (3)	O2^xiv—O3—O2ⁱⁱⁱ	150.47 (3)
O2—S—O2^v	108.95 (4)	Mg—O3—O1ⁱ	43.718 (13)
S—O1—Mg^vi	140.26 (3)	Mg^v—O3—O1ⁱ	106.01 (2)
S—O1—O2	35.968 (17)	O2^xiii—O3—O1ⁱ	71.144 (18)
Mg^vi—O1—O2	104.29 (2)	O2ⁱⁱ—O3—O1ⁱ	132.219 (16)
S—O1—O1^v	35.02 (2)	O2^xiv—O3—O1ⁱ	142.035 (17)
Mg^vi—O1—O1^v	144.98 (4)	O2ⁱⁱⁱ—O3—O1ⁱ	56.736 (16)
O2—O1—O1^v	60.66 (2)	Mg—O3—O1^vii	106.01 (2)
S—O1—O2^v	35.083 (17)	Mg^v—O3—O1^vii	43.718 (13)
Mg^vi—O1—O2^v	143.93 (3)	O2^xiii—O3—O1^vii	132.219 (16)
O2—O1—O2^v	60.21 (3)	O2ⁱⁱ—O3—O1^vii	71.144 (18)
O1^v—O1—O2^v	59.58 (2)	O2^xiv—O3—O1^vii	56.736 (16)
S—O1—O2^vi	131.90 (3)	O2ⁱⁱⁱ—O3—O1^vii	142.035 (17)
Mg^vi—O1—O2^vi	47.280 (15)	O1ⁱ—O3—O1^vii	123.86 (3)
O2—O1—O2^vi	112.81 (2)	Mg—O3—O1^xiii	121.59 (2)
O1^v—O1—O2^vi	106.26 (2)	Mg^v—O3—O1^xiii	42.271 (11)
O2^v—O1—O2^vi	165.74 (3)	O2^xiii—O3—O1^xiii	48.900 (14)
S—O1—O3^vii	166.64 (3)	O2ⁱⁱ—O3—O1^xiii	145.696 (16)
Mg^vi—O1—O3^vii	47.837 (12)	O2^xiv—O3—O1^xiii	60.349 (16)
O2—O1—O3^vii	149.14 (2)	O2ⁱⁱⁱ—O3—O1^xiii	127.643 (15)
O1^v—O1—O3^vii	149.12 (2)	O1ⁱ—O3—O1^xiii	81.706 (17)
O2^v—O1—O3^vii	131.56 (3)	O1^vii—O3—O1^xiii	85.990 (19)
O2^vi—O1—O3^vii	61.249 (17)	Mg—O3—O1ⁱⁱ	42.271 (11)
S—O1—O2^viii	115.09 (3)	Mg^v—O3—O1ⁱⁱ	121.59 (2)
Mg^vi—O1—O2^viii	43.216 (15)	O2^xiii—O3—O1ⁱⁱ	145.696 (16)
O2—O1—O2^viii	88.54 (2)	O2ⁱⁱ—O3—O1ⁱⁱ	48.900 (14)
O1^v—O1—O2^viii	148.607 (18)	O2^xiv—O3—O1ⁱⁱ	127.643 (15)
O2^v—O1—O2^viii	101.36 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	60.349 (16)
O2^vi—O1—O2^viii	90.50 (2)	O1ⁱ—O3—O1ⁱⁱ	85.990 (19)
O3^vii—O1—O2^viii	62.27 (2)	O1^vii—O3—O1ⁱⁱ	81.706 (17)
S—O1—O3^ix	95.04 (3)	O1^xiii—O3—O1ⁱⁱ	153.69 (3)
Mg^vi—O1—O3^ix	46.173 (14)	Mg—O3—O2	41.927 (14)
O2—O1—O3^ix	59.780 (19)	Mg^v—O3—O2	82.62 (2)
O1^v—O1—O3^ix	105.47 (3)	O2^xiii—O3—O2	125.35 (2)
O2^v—O1—O3^ix	116.24 (2)	O2ⁱⁱ—O3—O2	95.864 (14)
O2^vi—O1—O3^ix	63.59 (2)	O2^xiv—O3—O2	121.98 (2)
O3^vii—O1—O3^ix	94.010 (19)	O2ⁱⁱⁱ—O3—O2	86.481 (16)
O2^viii—O1—O3^ix	58.136 (17)	O1ⁱ—O3—O2	59.613 (18)
S—O1—O2^x	123.32 (3)	O1^vii—O3—O2	68.99 (2)
Mg^vi—O1—O2^x	96.263 (19)	O1^xiii—O3—O2	99.41 (2)
O2—O1—O2^x	158.87 (3)	O1ⁱⁱ—O3—O2	54.439 (15)
O1^v—O1—O2^x	99.37 (2)	Mg—O3—O2^v	82.62 (2)
O2^v—O1—O2^x	104.99 (2)	Mg^v—O3—O2^v	41.927 (14)
O2^vi—O1—O2^x	77.82 (2)	O2^xiii—O3—O2^v	95.864 (14)
O3^vii—O1—O2^x	51.832 (15)	O2ⁱⁱ—O3—O2^v	125.35 (2)
O2^viii—O1—O2^x	110.19 (2)	O2^xiv—O3—O2^v	86.481 (16)
O3^ix—O1—O2^x	138.44 (2)	O2ⁱⁱⁱ—O3—O2^v	121.98 (2)
S—O1—O3^xi	104.10 (3)	O1ⁱ—O3—O2^v	68.99 (2)
Mg^vi—O1—O3^xi	97.615 (19)	O1^vii—O3—O2^v	59.613 (18)
O2—O1—O3^xi	119.29 (2)	O1^xiii—O3—O2^v	54.439 (15)
O1^v—O1—O3^xi	69.078 (10)	O1ⁱⁱ—O3—O2^v	99.41 (2)
O2^v—O1—O3^xi	118.44 (2)	O2—O3—O2^v	46.59 (2)
O2^vi—O1—O3^xi	52.132 (16)	Mg—O3—H	107.0 (10)
O3^vii—O1—O3^xi	82.353 (17)	Mg^v—O3—H	107.9 (10)
O2^viii—O1—O3^xi	138.807 (18)	O2^xiii—O3—H	118.1 (10)
O3^ix—O1—O3^xi	107.93 (2)	O2ⁱⁱ—O3—H	20.2 (10)
O2^x—O1—O3^xi	51.750 (13)	O2^xiv—O3—H	72.3 (10)
S—O1—O2^vii	111.08 (3)	O2ⁱⁱⁱ—O3—H	88.9 (10)
Mg^vi—O1—O2^vii	76.290 (19)	O1ⁱ—O3—H	144.7 (10)
O2—O1—O2^vii	109.23 (2)	O1^vii—O3—H	77.2 (10)
O1^v—O1—O2^vii	137.22 (3)	O1^xiii—O3—H	131.3 (10)
O2^v—O1—O2^vii	79.032 (19)	O1ⁱⁱ—O3—H	68.1 (10)
O2^vi—O1—O2^vii	115.20 (2)	O2—O3—H	115.7 (10)
O3^vii—O1—O2^vii	57.239 (18)	O2^v—O3—H	136.5 (10)
O2^viii—O1—O2^vii	43.996 (18)	Mg—O3—H^v	107.9 (10)
O3^ix—O1—O2^vii	101.989 (19)	Mg^v—O3—H^v	107.0 (10)
O2^x—O1—O2^vii	80.142 (15)	O2^xiii—O3—H^v	20.2 (10)
O3^xi—O1—O2^vii	130.929 (17)	O2ⁱⁱ—O3—H^v	118.1 (10)
S—O2—Mg	134.16 (3)	O2^xiv—O3—H^v	88.9 (10)
S—O2—O1	35.430 (17)	O2ⁱⁱⁱ—O3—H^v	72.3 (10)
Mg—O2—O1	162.29 (3)	O1ⁱ—O3—H^v	77.2 (10)
S—O2—O2^v	35.52 (2)	O1^vii—O3—H^v	144.7 (10)
Mg—O2—O2^v	103.673 (18)	O1^xiii—O3—H^v	68.1 (10)
O1—O2—O2^v	60.43 (2)	O1ⁱⁱ—O3—H^v	131.3 (10)
S—O2—O1^v	34.563 (17)	O2—O3—H^v	136.5 (10)
Mg—O2—O1^v	120.97 (3)	O2^v—O3—H^v	115.7 (10)
O1—O2—O1^v	59.76 (3)	H—O3—H^v	102 (2)
O2^v—O2—O1^v	59.359 (19)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱ	0.816 (14)	1.996 (14)	2.7422 (6)	151.7 (14)

Symmetry code: (ii) −x+1/2, y+1/2, −z+1/2.

(MgSO4H2O_N2_313K) top

Crystal data top

Fe₀H₂MgO₅S	V = 355.94 (9) Å³
M_r = 138.39	Z = 4
Monoclinic, C2/c	F(000) = 280
a = 6.9227 (10) Å	D_x = 2.582 Mg m⁻³
b = 7.6212 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.6488 (10) Å	µ = 0.97 mm⁻¹
β = 118.112 (10)°	T = 313 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.021
T_min = 0.685, T_max = 0.748	θ_max = 40.0°, θ_min = 4.2°
9957 measured reflections	h = −12→12
1103 independent reflections	k = −13→13
1049 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.017	w = 1/[σ²(F_o²) + (0.020P)² + 0.220P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.048	(Δ/σ)_max < 0.001
S = 1.18	Δρ_max = 0.47 e Å⁻³
1103 reflections	Δρ_min = −0.37 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.004 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Mg	0.000000	0.500000	0.000000	0.00852 (7)
S	0.000000	0.15461 (3)	0.250000	0.00684 (5)
O1	0.17585 (8)	0.04442 (7)	0.39411 (8)	0.01380 (9)
O2	0.09120 (9)	0.26743 (7)	0.14908 (8)	0.01257 (9)
O3	0.000000	0.63534 (10)	0.250000	0.01125 (11)
H	0.103 (2)	0.703 (2)	0.293 (2)	0.028 (4)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mg	0.00750 (13)	0.00876 (13)	0.00858 (13)	−0.00057 (9)	0.00319 (10)	0.00055 (9)
S	0.00519 (8)	0.00655 (8)	0.00819 (8)	0.000	0.00267 (6)	0.000
O1	0.00842 (18)	0.0155 (2)	0.0157 (2)	0.00412 (15)	0.00418 (15)	0.00690 (16)
O2	0.0126 (2)	0.01123 (18)	0.0167 (2)	0.00131 (14)	0.00915 (17)	0.00498 (15)
O3	0.0110 (3)	0.0123 (3)	0.0110 (2)	0.000	0.0056 (2)	0.000

Geometric parameters (Å, º) top

Mg—O1ⁱ	2.0232 (6)	O1—O2	2.3895 (8)
Mg—O1ⁱⁱ	2.0232 (6)	O1—O1^v	2.3937 (11)
Mg—O2	2.0401 (5)	O1—O2^v	2.4166 (8)
Mg—O2ⁱⁱⁱ	2.0401 (5)	O1—O2^vi	2.7691 (8)
Mg—O3	2.1726 (4)	O1—O3^vii	2.9267 (7)
Mg—O3ⁱⁱⁱ	2.1726 (4)	O1—O2^viii	2.9736 (9)
Mg—O2ⁱ	3.4941 (7)	O1—O3^ix	3.0103 (7)
Mg—O2ⁱⁱ	3.4942 (7)	O1—O2^x	3.2973 (8)
Mg—O2^iv	3.5131 (6)	O1—O3^xi	3.3395 (10)
Mg—O2^v	3.5131 (6)	O1—O2^vii	3.3993 (9)
Mg—O1^iv	3.8888 (7)	O2—O2^v	2.4115 (11)
Mg—O1^v	3.8888 (7)	O2—O3^ix	2.7495 (7)
S—O1^v	1.4621 (5)	O2—O3ⁱⁱⁱ	2.9067 (7)
S—O1	1.4621 (5)	O2—O3	3.0521 (9)
S—O2^v	1.4809 (5)	O3—H	0.812 (15)
S—O2	1.4809 (5)	O3—H^v	0.812 (15)

O1ⁱ—Mg—O1ⁱⁱ	180.0	S—O2—O3^ix	106.04 (3)
O1ⁱ—Mg—O2	94.08 (2)	Mg—O2—O3^ix	118.79 (2)
O1ⁱⁱ—Mg—O2	85.92 (2)	O1—O2—O3^ix	71.32 (2)
O1ⁱ—Mg—O2ⁱⁱⁱ	85.92 (2)	O2^v—O2—O3^ix	126.90 (3)
O1ⁱⁱ—Mg—O2ⁱⁱⁱ	94.08 (2)	O1^v—O2—O3^ix	113.63 (3)
O2—Mg—O2ⁱⁱⁱ	180.0	S—O2—O1ⁱⁱ	156.94 (3)
O1ⁱ—Mg—O3	88.384 (18)	Mg—O2—O1ⁱⁱ	46.784 (17)
O1ⁱⁱ—Mg—O3	91.616 (18)	O1—O2—O1ⁱⁱ	133.98 (2)
O2—Mg—O3	92.80 (2)	O2^v—O2—O1ⁱⁱ	125.90 (2)
O2ⁱⁱⁱ—Mg—O3	87.20 (2)	O1^v—O2—O1ⁱⁱ	166.13 (3)
O1ⁱ—Mg—O3ⁱⁱⁱ	91.616 (18)	O3^ix—O2—O1ⁱⁱ	74.48 (2)
O1ⁱⁱ—Mg—O3ⁱⁱⁱ	88.384 (18)	S—O2—O3ⁱⁱⁱ	139.50 (3)
O2—Mg—O3ⁱⁱⁱ	87.20 (2)	Mg—O2—O3ⁱⁱⁱ	48.294 (18)
O2ⁱⁱⁱ—Mg—O3ⁱⁱⁱ	92.80 (2)	O1—O2—O3ⁱⁱⁱ	148.94 (3)
O3—Mg—O3ⁱⁱⁱ	180.0	O2^v—O2—O3ⁱⁱⁱ	138.78 (3)
O1ⁱ—Mg—O2ⁱ	41.480 (18)	O1^v—O2—O3ⁱⁱⁱ	105.20 (3)
O1ⁱⁱ—Mg—O2ⁱ	138.520 (18)	O3^ix—O2—O3ⁱⁱⁱ	94.23 (2)
O2—Mg—O2ⁱ	81.251 (14)	O1ⁱⁱ—O2—O3ⁱⁱⁱ	62.03 (2)
O2ⁱⁱⁱ—Mg—O2ⁱ	98.748 (14)	S—O2—O1ⁱ	95.96 (3)
O3—Mg—O2ⁱ	128.107 (13)	Mg—O2—O1ⁱ	42.738 (15)
O3ⁱⁱⁱ—Mg—O2ⁱ	51.893 (13)	O1—O2—O1ⁱ	131.40 (3)
O1ⁱ—Mg—O2ⁱⁱ	138.520 (18)	O2^v—O2—O1ⁱ	77.51 (3)
O1ⁱⁱ—Mg—O2ⁱⁱ	41.480 (18)	O1^v—O2—O1ⁱ	78.96 (3)
O2—Mg—O2ⁱⁱ	98.749 (13)	O3^ix—O2—O1ⁱ	155.50 (2)
O2ⁱⁱⁱ—Mg—O2ⁱⁱ	81.252 (14)	O1ⁱⁱ—O2—O1ⁱ	89.52 (2)
O3—Mg—O2ⁱⁱ	51.893 (14)	O3ⁱⁱⁱ—O2—O1ⁱ	61.571 (18)
O3ⁱⁱⁱ—Mg—O2ⁱⁱ	128.107 (13)	S—O2—O3	102.22 (3)
O2ⁱ—Mg—O2ⁱⁱ	180.0	Mg—O2—O3	45.316 (14)
O1ⁱ—Mg—O2^iv	110.08 (2)	O1—O2—O3	117.29 (3)
O1ⁱⁱ—Mg—O2^iv	69.92 (2)	O2^v—O2—O3	66.731 (11)
O2—Mg—O2^iv	138.22 (2)	O1^v—O2—O3	116.40 (2)
O2ⁱⁱⁱ—Mg—O2^iv	41.78 (2)	O3^ix—O2—O3	125.00 (2)
O3—Mg—O2^iv	120.50 (2)	O1ⁱⁱ—O2—O3	62.053 (18)
O3ⁱⁱⁱ—Mg—O2^iv	59.51 (2)	O3ⁱⁱⁱ—O2—O3	93.609 (18)
O2ⁱ—Mg—O2^iv	94.558 (17)	O1ⁱ—O2—O3	58.099 (15)
O2ⁱⁱ—Mg—O2^iv	85.443 (17)	S—O2—O1^xii	97.36 (3)
O1ⁱ—Mg—O2^v	69.92 (2)	Mg—O2—O1^xii	112.96 (2)
O1ⁱⁱ—Mg—O2^v	110.08 (2)	O1—O2—O1^xii	84.547 (18)
O2—Mg—O2^v	41.783 (19)	O2^v—O2—O1^xii	132.165 (16)
O2ⁱⁱⁱ—Mg—O2^v	138.217 (19)	O1^v—O2—O1^xii	75.52 (2)
O3—Mg—O2^v	59.50 (2)	O3^ix—O2—O1^xii	57.035 (18)
O3ⁱⁱⁱ—Mg—O2^v	120.49 (2)	O1ⁱⁱ—O2—O1^xii	101.72 (2)
O2ⁱ—Mg—O2^v	85.442 (17)	O3ⁱⁱⁱ—O2—O1^xii	64.78 (2)
O2ⁱⁱ—Mg—O2^v	94.557 (17)	O1ⁱ—O2—O1^xii	110.25 (2)
O2^iv—Mg—O2^v	180.000 (11)	O3—O2—O1^xii	158.03 (2)
O1ⁱ—Mg—O1^iv	117.58 (2)	S—O2—O1^vii	79.71 (3)
O1ⁱⁱ—Mg—O1^iv	62.42 (2)	Mg—O2—O1^vii	94.59 (2)
O2—Mg—O1^iv	147.922 (18)	O1—O2—O1^vii	70.83 (3)
O2ⁱⁱⁱ—Mg—O1^iv	32.079 (18)	O2^v—O2—O1^vii	58.66 (2)
O3—Mg—O1^iv	83.64 (2)	O1^v—O2—O1^vii	113.52 (3)
O3ⁱⁱⁱ—Mg—O1^iv	96.36 (2)	O3^ix—O2—O1^vii	86.49 (2)
O2ⁱ—Mg—O1^iv	125.488 (14)	O1ⁱⁱ—O2—O1^vii	77.300 (18)
O2ⁱⁱ—Mg—O1^iv	54.512 (14)	O3ⁱⁱⁱ—O2—O1^vii	137.31 (2)
O2^iv—Mg—O1^iv	37.232 (12)	O1ⁱ—O2—O1^vii	108.33 (2)
O2^v—Mg—O1^iv	142.768 (12)	O3—O2—O1^vii	53.629 (14)
O1ⁱ—Mg—O1^v	62.42 (2)	O1^xii—O2—O1^vii	141.40 (2)
O1ⁱⁱ—Mg—O1^v	117.58 (2)	Mg—O3—Mg^v	123.32 (4)
O2—Mg—O1^v	32.078 (18)	Mg—O3—O2^xiii	110.707 (16)
O2ⁱⁱⁱ—Mg—O1^v	147.921 (18)	Mg^v—O3—O2^xiii	89.660 (14)
O3—Mg—O1^v	96.36 (2)	Mg—O3—O2ⁱⁱ	89.660 (14)
O3ⁱⁱⁱ—Mg—O1^v	83.64 (2)	Mg^v—O3—O2ⁱⁱ	110.706 (16)
O2ⁱ—Mg—O1^v	54.512 (14)	O2^xiii—O3—O2ⁱⁱ	137.04 (4)
O2ⁱⁱ—Mg—O1^v	125.488 (14)	Mg—O3—O2^xiv	162.78 (3)
O2^iv—Mg—O1^v	142.768 (12)	Mg^v—O3—O2^xiv	44.508 (13)
O2^v—Mg—O1^v	37.232 (12)	O2^xiii—O3—O2^xiv	83.512 (18)
O1^iv—Mg—O1^v	180.0	O2ⁱⁱ—O3—O2^xiv	85.77 (2)
O1^v—S—O1	109.89 (5)	Mg—O3—O2ⁱⁱⁱ	44.508 (13)
O1^v—S—O2^v	108.57 (3)	Mg^v—O3—O2ⁱⁱⁱ	162.78 (3)
O1—S—O2^v	110.40 (3)	O2^xiii—O3—O2ⁱⁱⁱ	85.77 (2)
O1^v—S—O2	110.40 (3)	O2ⁱⁱ—O3—O2ⁱⁱⁱ	83.513 (18)
O1—S—O2	108.57 (3)	O2^xiv—O3—O2ⁱⁱⁱ	150.46 (4)
O2^v—S—O2	109.01 (4)	Mg—O3—O1ⁱ	43.710 (14)
S—O1—Mg^vi	140.38 (4)	Mg^v—O3—O1ⁱ	106.17 (3)
S—O1—O2	35.979 (19)	O2^xiii—O3—O1ⁱ	70.950 (19)
Mg^vi—O1—O2	104.41 (3)	O2ⁱⁱ—O3—O1ⁱ	132.004 (17)
S—O1—O1^v	35.06 (2)	O2^xiv—O3—O1ⁱ	142.000 (19)
Mg^vi—O1—O1^v	145.45 (4)	O2ⁱⁱⁱ—O3—O1ⁱ	56.677 (18)
O2—O1—O1^v	60.69 (2)	Mg—O3—O1^vii	106.17 (3)
S—O1—O2^v	35.06 (2)	Mg^v—O3—O1^vii	43.710 (14)
Mg^vi—O1—O2^v	143.63 (3)	O2^xiii—O3—O1^vii	132.004 (17)
O2—O1—O2^v	60.23 (3)	O2ⁱⁱ—O3—O1^vii	70.949 (19)
O1^v—O1—O2^v	59.57 (2)	O2^xiv—O3—O1^vii	56.677 (18)
S—O1—O2^vi	132.28 (4)	O2ⁱⁱⁱ—O3—O1^vii	142.000 (19)
Mg^vi—O1—O2^vi	47.296 (16)	O1ⁱ—O3—O1^vii	124.18 (4)
O2—O1—O2^vi	112.96 (2)	Mg—O3—O1^xiii	121.48 (2)
O1^v—O1—O2^vi	106.67 (3)	Mg^v—O3—O1^xiii	42.209 (12)
O2^v—O1—O2^vi	166.13 (3)	O2^xiii—O3—O1^xiii	48.763 (16)
S—O1—O3^vii	166.21 (4)	O2ⁱⁱ—O3—O1^xiii	145.867 (18)
Mg^vi—O1—O3^vii	47.907 (13)	O2^xiv—O3—O1^xiii	60.309 (17)
O2—O1—O3^vii	149.28 (3)	O2ⁱⁱⁱ—O3—O1^xiii	127.784 (17)
O1^v—O1—O3^vii	149.09 (2)	O1ⁱ—O3—O1^xiii	81.702 (18)
O2^v—O1—O3^vii	131.17 (3)	O1^vii—O3—O1^xiii	85.92 (2)
O2^vi—O1—O3^vii	61.297 (19)	Mg—O3—O1ⁱⁱ	42.209 (12)
S—O1—O2^viii	114.95 (3)	Mg^v—O3—O1ⁱⁱ	121.48 (2)
Mg^vi—O1—O2^viii	43.182 (16)	O2^xiii—O3—O1ⁱⁱ	145.867 (18)
O2—O1—O2^viii	88.59 (2)	O2ⁱⁱ—O3—O1ⁱⁱ	48.764 (16)
O1^v—O1—O2^viii	148.61 (2)	O2^xiv—O3—O1ⁱⁱ	127.784 (17)
O2^v—O1—O2^viii	101.04 (3)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	60.309 (17)
O2^vi—O1—O2^viii	90.48 (2)	O1ⁱ—O3—O1ⁱⁱ	85.92 (2)
O3^vii—O1—O2^viii	62.29 (2)	O1^vii—O3—O1ⁱⁱ	81.702 (18)
S—O1—O3^ix	95.24 (3)	O1^xiii—O3—O1ⁱⁱ	153.38 (4)
Mg^vi—O1—O3^ix	46.175 (15)	Mg—O3—O2^v	82.66 (2)
O2—O1—O3^ix	59.91 (2)	Mg^v—O3—O2^v	41.883 (16)
O1^v—O1—O3^ix	105.84 (3)	O2^xiii—O3—O2^v	95.691 (15)
O2^v—O1—O3^ix	116.25 (3)	O2ⁱⁱ—O3—O2^v	125.00 (2)
O2^vi—O1—O3^ix	63.59 (2)	O2^xiv—O3—O2^v	86.391 (18)
O3^vii—O1—O3^ix	94.08 (2)	O2ⁱⁱⁱ—O3—O2^v	122.10 (2)
O2^viii—O1—O3^ix	58.121 (18)	O1ⁱ—O3—O2^v	69.26 (2)
S—O1—O2^x	122.89 (3)	O1^vii—O3—O2^v	59.61 (2)
Mg^vi—O1—O2^x	96.62 (2)	O1^xiii—O3—O2^v	54.352 (16)
O2—O1—O2^x	158.49 (3)	O1ⁱⁱ—O3—O2^v	99.20 (2)
O1^v—O1—O2^x	99.07 (2)	Mg—O3—O2	41.883 (16)
O2^v—O1—O2^x	104.48 (2)	Mg^v—O3—O2	82.66 (2)
O2^vi—O1—O2^x	78.28 (2)	O2^xiii—O3—O2	125.00 (3)
O3^vii—O1—O2^x	52.016 (17)	O2ⁱⁱ—O3—O2	95.691 (15)
O2^viii—O1—O2^x	110.25 (2)	O2^xiv—O3—O2	122.10 (2)
O3^ix—O1—O2^x	138.88 (2)	O2ⁱⁱⁱ—O3—O2	86.391 (18)
S—O1—O3^xi	104.05 (3)	O1ⁱ—O3—O2	59.61 (2)
Mg^vi—O1—O3^xi	97.99 (2)	O1^vii—O3—O2	69.26 (2)
O2—O1—O3^xi	119.25 (3)	O1^xiii—O3—O2	99.20 (2)
O1^v—O1—O3^xi	68.998 (11)	O1ⁱⁱ—O3—O2	54.352 (16)
O2^v—O1—O3^xi	118.36 (2)	O2^v—O3—O2	46.54 (2)
O2^vi—O1—O3^xi	52.493 (17)	Mg—O3—H	106.9 (11)
O3^vii—O1—O3^xi	82.559 (18)	Mg^v—O3—H	107.9 (11)
O2^viii—O1—O3^xi	139.12 (2)	O2^xiii—O3—H	118.4 (11)
O3^ix—O1—O3^xi	108.22 (2)	O2ⁱⁱ—O3—H	20.4 (11)
O2^x—O1—O3^xi	51.944 (14)	O2^xiv—O3—H	72.5 (11)
S—O1—O2^vii	110.85 (3)	O2ⁱⁱⁱ—O3—H	88.8 (11)
Mg^vi—O1—O2^vii	76.09 (2)	O1ⁱ—O3—H	144.6 (11)
O2—O1—O2^vii	109.17 (3)	O1^vii—O3—H	77.0 (11)
O1^v—O1—O2^vii	136.95 (3)	O1^xiii—O3—H	131.4 (11)
O2^v—O1—O2^vii	78.80 (2)	O1ⁱⁱ—O3—H	68.2 (11)
O2^vi—O1—O2^vii	115.04 (3)	O2^v—O3—H	136.4 (11)
O3^vii—O1—O2^vii	57.11 (2)	O2—O3—H	115.8 (11)
O2^viii—O1—O2^vii	43.84 (2)	Mg—O3—H^v	107.9 (11)
O3^ix—O1—O2^vii	101.82 (2)	Mg^v—O3—H^v	106.9 (11)
O2^x—O1—O2^vii	80.012 (17)	O2^xiii—O3—H^v	20.4 (11)
O3^xi—O1—O2^vii	130.971 (19)	O2ⁱⁱ—O3—H^v	118.4 (11)
S—O2—Mg	134.44 (3)	O2^xiv—O3—H^v	88.8 (11)
S—O2—O1	35.452 (19)	O2ⁱⁱⁱ—O3—H^v	72.5 (11)
Mg—O2—O1	162.42 (3)	O1ⁱ—O3—H^v	77.0 (11)
S—O2—O2^v	35.49 (2)	O1^vii—O3—H^v	144.6 (11)
Mg—O2—O2^v	103.91 (2)	O1^xiii—O3—H^v	68.2 (11)
O1—O2—O2^v	60.44 (2)	O1ⁱⁱ—O3—H^v	131.4 (11)
S—O2—O1^v	34.546 (19)	O2^v—O3—H^v	115.8 (11)
Mg—O2—O1^v	121.29 (3)	O2—O3—H^v	136.4 (11)
O1—O2—O1^v	59.74 (3)	H—O3—H^v	102 (2)
O2^v—O2—O1^v	59.33 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱ	0.812 (15)	2.008 (15)	2.7495 (7)	151.5 (15)

Symmetry code: (ii) −x+1/2, y+1/2, −z+1/2.

(FeSO4H2O_He_45K) top

Crystal data top

FeH₂O₅S	Z = 4
M_r = 169.93	F(000) = 336
Monoclinic, C2/c	D_x = 3.110 Mg m⁻³
a = 7.0304 (8) Å	Mo Kα radiation, λ = 0.71073 Å
b = 7.5789 (6) Å	µ = 4.61 mm⁻¹
c = 7.7374 (8) Å	T = 45 K
β = 118.314 (14)°	0.32 × 0.29 × 0.07 mm
V = 362.94 (8) Å³

Data collection top

1187 measured reflections	θ_max = 29.4°, θ_min = 4.2°
442 independent reflections	h = −9→9
425 reflections with I > 2σ(I)	k = −9→9
R_int = 0.020	l = −7→10

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.017	w = 1/[σ²(F_o²) + (0.021P)² + 0.040P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.042	(Δ/σ)_max < 0.001
S = 1.12	Δρ_max = 0.54 e Å⁻³
442 reflections	Δρ_min = −0.46 e Å⁻³
40 parameters	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0346 (18)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe	0.000000	0.500000	0.000000	0.00235 (16)
S	0.000000	0.15535 (7)	0.250000	0.00229 (17)
O1	0.1683 (2)	0.04564 (17)	0.40068 (17)	0.0046 (3)
O2	0.10045 (19)	0.27064 (15)	0.15967 (16)	0.0044 (3)
O3	0.000000	0.6435 (2)	0.250000	0.0045 (4)
H	0.101 (4)	0.715 (3)	0.290 (3)	0.020 (6)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe	0.0025 (2)	0.0022 (2)	0.0022 (2)	0.00025 (12)	0.00098 (16)	0.00075 (11)
S	0.0019 (3)	0.0024 (3)	0.0026 (3)	0.000	0.0011 (2)	0.000
O1	0.0036 (7)	0.0049 (6)	0.0045 (5)	0.0010 (5)	0.0013 (5)	0.0008 (5)
O2	0.0038 (7)	0.0042 (6)	0.0052 (5)	0.0002 (5)	0.0023 (5)	0.0017 (4)
O3	0.0036 (10)	0.0045 (9)	0.0056 (8)	0.000	0.0024 (7)	0.000

Geometric parameters (Å, º) top

Fe—O2ⁱ	2.0540 (11)	O1—O1^iv	2.409 (3)
Fe—O2	2.0540 (11)	O1—O2^iv	2.4204 (17)
Fe—O1ⁱⁱ	2.1093 (13)	O1—O2^vi	2.8153 (17)
Fe—O1ⁱⁱⁱ	2.1093 (13)	O1—O3^vii	2.9699 (15)
Fe—O3ⁱ	2.2193 (9)	O1—O2^viii	3.0676 (18)
Fe—O3	2.2193 (9)	O1—O3^ix	3.1509 (13)
Fe—O2ⁱⁱⁱ	3.4663 (13)	O1—O3^x	3.277 (2)
Fe—O2ⁱⁱ	3.4663 (13)	O1—O2^xi	3.3008 (16)
Fe—O2^iv	3.4955 (11)	O1—O2^vii	3.3026 (17)
Fe—O2^v	3.4955 (11)	O2—O2^iv	2.413 (2)
S—O1^iv	1.4635 (13)	O2—O3^ix	2.7285 (14)
S—O1	1.4635 (13)	O2—O3ⁱ	2.9742 (12)
S—O2	1.4896 (11)	O2—O3	3.0729 (19)
S—O2^iv	1.4896 (11)	O3—H	0.82 (2)
O1—O2	2.4019 (17)	O3—H^iv	0.82 (2)

O2ⁱ—Fe—O2	180.0	O3^ix—O2—O1ⁱⁱⁱ	72.45 (5)
O2ⁱ—Fe—O1ⁱⁱ	85.09 (5)	S—O2—O3ⁱ	134.63 (7)
O2—Fe—O1ⁱⁱ	94.91 (5)	Fe—O2—O3ⁱ	48.23 (4)
O2ⁱ—Fe—O1ⁱⁱⁱ	94.91 (5)	O1—O2—O3ⁱ	147.36 (7)
O2—Fe—O1ⁱⁱⁱ	85.09 (5)	O2^iv—O2—O3ⁱ	135.16 (7)
O1ⁱⁱ—Fe—O1ⁱⁱⁱ	180.00 (7)	O1^iv—O2—O3ⁱ	100.34 (5)
O2ⁱ—Fe—O3ⁱ	91.87 (5)	O3^ix—O2—O3ⁱ	92.60 (4)
O2—Fe—O3ⁱ	88.13 (5)	O1ⁱⁱⁱ—O2—O3ⁱ	61.65 (4)
O1ⁱⁱ—Fe—O3ⁱ	93.39 (3)	S—O2—O1ⁱⁱ	91.70 (6)
O1ⁱⁱⁱ—Fe—O3ⁱ	86.61 (3)	Fe—O2—O1ⁱⁱ	43.24 (3)
O2ⁱ—Fe—O3	88.12 (5)	O1—O2—O1ⁱⁱ	126.85 (7)
O2—Fe—O3	91.88 (5)	O2^iv—O2—O1ⁱⁱ	73.01 (5)
O1ⁱⁱ—Fe—O3	86.61 (3)	O1^iv—O2—O1ⁱⁱ	75.71 (6)
O1ⁱⁱⁱ—Fe—O3	93.39 (3)	O3^ix—O2—O1ⁱⁱ	155.23 (5)
O3ⁱ—Fe—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	91.53 (5)
O2ⁱ—Fe—O2ⁱⁱⁱ	83.09 (2)	O3ⁱ—O2—O1ⁱⁱ	62.85 (4)
O2—Fe—O2ⁱⁱⁱ	96.91 (2)	S—O2—O3	102.80 (6)
O1ⁱⁱ—Fe—O2ⁱⁱⁱ	137.00 (4)	Fe—O2—O3	46.21 (2)
O1ⁱⁱⁱ—Fe—O2ⁱⁱⁱ	43.00 (4)	O1—O2—O3	117.31 (5)
O3ⁱ—Fe—O2ⁱⁱⁱ	128.11 (3)	O2^iv—O2—O3	66.88 (2)
O3—Fe—O2ⁱⁱⁱ	51.89 (3)	O1^iv—O2—O3	116.70 (5)
O2ⁱ—Fe—O2ⁱⁱ	96.91 (2)	O3^ix—O2—O3	125.89 (6)
O2—Fe—O2ⁱⁱ	83.09 (2)	O1ⁱⁱⁱ—O2—O3	64.53 (4)
O1ⁱⁱ—Fe—O2ⁱⁱ	43.00 (4)	O3ⁱ—O2—O3	94.43 (4)
O1ⁱⁱⁱ—Fe—O2ⁱⁱ	137.00 (4)	O1ⁱⁱ—O2—O3	57.85 (3)
O3ⁱ—Fe—O2ⁱⁱ	51.89 (3)	S—O2—O1^xii	95.51 (6)
O3—Fe—O2ⁱⁱ	128.11 (3)	Fe—O2—O1^xii	110.91 (5)
O2ⁱⁱⁱ—Fe—O2ⁱⁱ	180.0	O1—O2—O1^xii	85.59 (3)
O2ⁱ—Fe—O2^iv	137.67 (4)	O2^iv—O2—O1^xii	130.13 (4)
O2—Fe—O2^iv	42.33 (4)	O1^iv—O2—O1^xii	72.27 (5)
O1ⁱⁱ—Fe—O2^iv	67.01 (4)	O3^ix—O2—O1^xii	58.10 (4)
O1ⁱⁱⁱ—Fe—O2^iv	112.99 (4)	O1ⁱⁱⁱ—O2—O1^xii	100.13 (4)
O3ⁱ—Fe—O2^iv	119.76 (4)	O3ⁱ—O2—O1^xii	62.71 (4)
O3—Fe—O2^iv	60.24 (4)	O1ⁱⁱ—O2—O1^xii	108.45 (5)
O2ⁱⁱⁱ—Fe—O2^iv	95.88 (3)	O3—O2—O1^xii	157.06 (4)
O2ⁱⁱ—Fe—O2^iv	84.12 (3)	S—O2—O1^vii	82.84 (5)
O2ⁱ—Fe—O2^v	42.33 (4)	Fe—O2—O1^vii	97.10 (4)
O2—Fe—O2^v	137.67 (4)	O1—O2—O1^vii	71.35 (5)
O1ⁱⁱ—Fe—O2^v	112.99 (4)	O2^iv—O2—O1^vii	62.66 (5)
O1ⁱⁱⁱ—Fe—O2^v	67.01 (4)	O1^iv—O2—O1^vii	116.98 (5)
O3ⁱ—Fe—O2^v	60.24 (4)	O3^ix—O2—O1^vii	86.61 (4)
O3—Fe—O2^v	119.76 (4)	O1ⁱⁱⁱ—O2—O1^vii	79.50 (4)
O2ⁱⁱⁱ—Fe—O2^v	84.12 (3)	O3ⁱ—O2—O1^vii	139.25 (5)
O2ⁱⁱ—Fe—O2^v	95.88 (3)	O1ⁱⁱ—O2—O1^vii	109.43 (5)
O2^iv—Fe—O2^v	180.00 (3)	O3—O2—O1^vii	55.39 (3)
O1^iv—S—O1	110.76 (11)	O1^xii—O2—O1^vii	142.11 (4)
O1^iv—S—O2	110.09 (6)	Fe—O3—Fe^iv	121.29 (8)
O1—S—O2	108.85 (7)	Fe—O3—O2ⁱⁱⁱ	88.32 (2)
O1^iv—S—O2^iv	108.85 (7)	Fe^iv—O3—O2ⁱⁱⁱ	112.05 (3)
O1—S—O2^iv	110.09 (6)	Fe—O3—O2^xiii	112.05 (3)
O2—S—O2^iv	108.17 (9)	Fe^iv—O3—O2^xiii	88.32 (3)
S—O1—Fe^vi	136.03 (7)	O2ⁱⁱⁱ—O3—O2^xiii	138.65 (8)
S—O1—O2	35.94 (4)	Fe—O3—O1ⁱⁱ	45.15 (3)
Fe^vi—O1—O2	100.21 (6)	Fe^iv—O3—O1ⁱⁱ	103.41 (6)
S—O1—O1^iv	34.62 (5)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	132.24 (4)
Fe^vi—O1—O1^iv	139.58 (8)	O2^xiii—O3—O1ⁱⁱ	70.65 (4)
O2—O1—O1^iv	60.41 (5)	Fe—O3—O1^vii	103.41 (6)
S—O1—O2^iv	35.31 (4)	Fe^iv—O3—O1^vii	45.15 (3)
Fe^vi—O1—O2^iv	144.37 (7)	O2ⁱⁱⁱ—O3—O1^vii	70.65 (4)
O2—O1—O2^iv	60.04 (6)	O2^xiii—O3—O1^vii	132.24 (4)
O1^iv—O1—O2^iv	59.66 (5)	O1ⁱⁱ—O3—O1^vii	122.27 (8)
S—O1—O2^vi	126.92 (7)	Fe—O3—O2^xiv	159.71 (6)
Fe^vi—O1—O2^vi	46.63 (3)	Fe^iv—O3—O2^xiv	43.65 (2)
O2—O1—O2^vi	108.32 (4)	O2ⁱⁱⁱ—O3—O2^xiv	87.40 (4)
O1^iv—O1—O2^vi	102.64 (5)	O2^xiii—O3—O2^xiv	83.74 (4)
O2^iv—O1—O2^vi	161.61 (7)	O1ⁱⁱ—O3—O2^xiv	139.68 (4)
S—O1—O3^vii	171.27 (7)	O1^vii—O3—O2^xiv	56.54 (3)
Fe^vi—O1—O3^vii	48.24 (3)	Fe—O3—O2ⁱ	43.65 (2)
O2—O1—O3^vii	146.13 (6)	Fe^iv—O3—O2ⁱ	159.71 (6)
O1^iv—O1—O3^vii	150.20 (4)	O2ⁱⁱⁱ—O3—O2ⁱ	83.74 (3)
O2^iv—O1—O3^vii	136.04 (5)	O2^xiii—O3—O2ⁱ	87.40 (4)
O2^vi—O1—O3^vii	61.81 (4)	O1ⁱⁱ—O3—O2ⁱ	56.54 (3)
S—O1—O2^viii	116.01 (7)	O1^vii—O3—O2ⁱ	139.68 (4)
Fe^vi—O1—O2^viii	41.84 (3)	O2^xiv—O3—O2ⁱ	154.74 (8)
O2—O1—O2^viii	87.44 (5)	Fe—O3—O2^iv	80.93 (6)
O1^iv—O1—O2^viii	147.80 (5)	Fe^iv—O3—O2^iv	41.92 (3)
O2^iv—O1—O2^viii	104.29 (6)	O2ⁱⁱⁱ—O3—O2^iv	125.89 (6)
O2^vi—O1—O2^viii	88.47 (5)	O2^xiii—O3—O2^iv	93.63 (3)
O3^vii—O1—O2^viii	61.16 (4)	O1ⁱⁱ—O3—O2^iv	66.23 (5)
S—O1—O3^ix	91.83 (5)	O1^vii—O3—O2^iv	60.99 (4)
Fe^vi—O1—O3^ix	44.68 (3)	O2^xiv—O3—O2^iv	85.57 (4)
O2—O1—O3^ix	56.96 (4)	O2ⁱ—O3—O2^iv	118.65 (5)
O1^iv—O1—O3^ix	101.62 (6)	Fe—O3—O2	41.92 (3)
O2^iv—O1—O3^ix	114.18 (6)	Fe^iv—O3—O2	80.93 (6)
O2^vi—O1—O3^ix	61.70 (4)	O2ⁱⁱⁱ—O3—O2	93.62 (3)
O3^vii—O1—O3^ix	92.92 (4)	O2^xiii—O3—O2	125.89 (6)
O2^viii—O1—O3^ix	57.13 (3)	O1ⁱⁱ—O3—O2	60.99 (4)
S—O1—O3^x	103.06 (6)	O1^vii—O3—O2	66.23 (5)
Fe^vi—O1—O3^x	97.31 (4)	O2^xiv—O3—O2	118.65 (5)
O2—O1—O3^x	118.61 (5)	O2ⁱ—O3—O2	85.57 (4)
O1^iv—O1—O3^x	68.44 (3)	O2^iv—O3—O2	46.23 (5)
O2^iv—O1—O3^x	118.01 (6)	Fe—O3—O1^xiii	120.87 (5)
O2^vi—O1—O3^x	52.55 (4)	Fe^iv—O3—O1^xiii	41.93 (2)
O3^vii—O1—O3^x	82.53 (4)	O2ⁱⁱⁱ—O3—O1^xiii	147.26 (3)
O2^viii—O1—O3^x	137.15 (5)	O2^xiii—O3—O1^xiii	47.56 (3)
O3^ix—O1—O3^x	107.04 (5)	O1ⁱⁱ—O3—O1^xiii	79.83 (4)
S—O1—O2^xi	126.96 (7)	O1^vii—O3—O1^xiii	87.09 (4)
Fe^vi—O1—O2^xi	96.48 (5)	O2^xiv—O3—O1^xiii	60.03 (3)
O2—O1—O2^xi	162.61 (7)	O2ⁱ—O3—O1^xiii	127.05 (3)
O1^iv—O1—O2^xi	103.26 (5)	O2^iv—O3—O1^xiii	53.77 (4)
O2^iv—O1—O2^xi	107.73 (5)	O2—O3—O1^xiii	99.08 (5)
O2^vi—O1—O2^xi	79.87 (4)	Fe—O3—O1ⁱⁱⁱ	41.93 (2)
O3^vii—O1—O2^xi	51.25 (3)	Fe^iv—O3—O1ⁱⁱⁱ	120.87 (5)
O2^viii—O1—O2^xi	108.46 (5)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	47.56 (3)
O3^ix—O1—O2^xi	137.82 (5)	O2^xiii—O3—O1ⁱⁱⁱ	147.26 (3)
O3^x—O1—O2^xi	53.76 (3)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	87.09 (4)
S—O1—O2^vii	113.46 (6)	O1^vii—O3—O1ⁱⁱⁱ	79.83 (4)
Fe^vi—O1—O2^vii	76.98 (4)	O2^xiv—O3—O1ⁱⁱⁱ	127.05 (3)
O2—O1—O2^vii	108.65 (5)	O2ⁱ—O3—O1ⁱⁱⁱ	60.03 (3)
O1^iv—O1—O2^vii	140.79 (6)	O2^iv—O3—O1ⁱⁱⁱ	99.08 (5)
O2^iv—O1—O2^vii	81.93 (4)	O2—O3—O1ⁱⁱⁱ	53.77 (4)
O2^vi—O1—O2^vii	116.23 (6)	O1^xiii—O3—O1ⁱⁱⁱ	152.76 (8)
O3^vii—O1—O2^vii	58.38 (4)	Fe—O3—H	107.0 (15)
O2^viii—O1—O2^vii	44.32 (4)	Fe^iv—O3—H	110.3 (15)
O3^ix—O1—O2^vii	101.11 (4)	O2ⁱⁱⁱ—O3—H	22.5 (16)
O3^x—O1—O2^vii	132.60 (4)	O2^xiii—O3—H	117.5 (16)
O2^xi—O1—O2^vii	79.81 (3)	O1ⁱⁱ—O3—H	145.2 (15)
S—O2—Fe	132.41 (7)	O1^vii—O3—H	79.0 (16)
S—O2—O1	35.21 (4)	O2^xiv—O3—H	74.3 (15)
Fe—O2—O1	162.33 (7)	O2ⁱ—O3—H	89.2 (15)
S—O2—O2^iv	35.92 (5)	O2^iv—O3—H	139.8 (16)
Fe—O2—O2^iv	102.69 (5)	O2—O3—H	115.9 (16)
O1—O2—O2^iv	60.36 (5)	O1^xiii—O3—H	132.0 (15)
S—O2—O1^iv	34.60 (4)	O1ⁱⁱⁱ—O3—H	68.8 (16)
Fe—O2—O1^iv	117.77 (6)	Fe—O3—H^iv	110.3 (15)
O1—O2—O1^iv	59.93 (7)	Fe^iv—O3—H^iv	107.0 (15)
O2^iv—O2—O1^iv	59.60 (5)	O2ⁱⁱⁱ—O3—H^iv	117.5 (16)
S—O2—O3^ix	109.41 (6)	O2^xiii—O3—H^iv	22.5 (16)
Fe—O2—O3^ix	118.12 (6)	O1ⁱⁱ—O3—H^iv	79.0 (16)
O1—O2—O3^ix	75.48 (5)	O1^vii—O3—H^iv	145.2 (15)
O2^iv—O2—O3^ix	131.76 (6)	O2^xiv—O3—H^iv	89.2 (15)
O1^iv—O2—O3^ix	114.53 (6)	O2ⁱ—O3—H^iv	74.3 (15)
S—O2—O1ⁱⁱⁱ	162.12 (7)	O2^iv—O3—H^iv	115.9 (16)
Fe—O2—O1ⁱⁱⁱ	48.29 (4)	O2—O3—H^iv	139.8 (16)
O1—O2—O1ⁱⁱⁱ	137.46 (5)	O1^xiii—O3—H^iv	68.8 (16)
O2^iv—O2—O1ⁱⁱⁱ	129.71 (4)	O1ⁱⁱⁱ—O3—H^iv	132.0 (15)
O1^iv—O2—O1ⁱⁱⁱ	161.61 (7)	H—O3—H^iv	98 (3)

O1^iv—S—O1—Fe^vi	115.38 (11)	O2^iv—S—O2—Fe	−41.09 (6)
O2—S—O1—Fe^vi	−5.78 (13)	O1^iv—S—O2—O1	−121.57 (10)
O2^iv—S—O1—Fe^vi	−124.19 (10)	O2^iv—S—O2—O1	119.60 (6)
O1^iv—S—O1—O2	121.17 (6)	O1^iv—S—O2—O2^iv	118.82 (6)
O2^iv—S—O1—O2	−118.40 (9)	O1—S—O2—O2^iv	−119.60 (6)
O2—S—O1—O1^iv	−121.17 (6)	O1—S—O2—O1^iv	121.57 (10)
O2^iv—S—O1—O1^iv	120.43 (6)	O2^iv—S—O2—O1^iv	−118.82 (6)
O1^iv—S—O1—O2^iv	−120.43 (6)	O1^iv—S—O2—O3^ix	−105.34 (7)
O2—S—O1—O2^iv	118.40 (9)	O1—S—O2—O3^ix	16.24 (8)
O1^iv—S—O1—O2^vi	52.66 (7)	O2^iv—S—O2—O3^ix	135.84 (7)
O2—S—O1—O2^vi	−68.50 (9)	O1^iv—S—O2—O1ⁱⁱⁱ	161.8 (3)
O2^iv—S—O1—O2^vi	173.10 (10)	O1—S—O2—O1ⁱⁱⁱ	−76.7 (2)
O1^iv—S—O1—O2^viii	161.90 (8)	O2^iv—S—O2—O1ⁱⁱⁱ	42.9 (2)
O2—S—O1—O2^viii	40.73 (8)	O1^iv—S—O2—O3ⁱ	9.21 (12)
O2^iv—S—O1—O2^viii	−77.67 (8)	O1—S—O2—O3ⁱ	130.78 (10)
O1^iv—S—O1—O3^ix	107.96 (5)	O2^iv—S—O2—O3ⁱ	−109.61 (10)
O2—S—O1—O3^ix	−13.21 (7)	O1^iv—S—O2—O1ⁱⁱ	61.45 (8)
O2^iv—S—O1—O3^ix	−131.61 (6)	O1—S—O2—O1ⁱⁱ	−176.97 (6)
O1^iv—S—O1—O3^x	0.000 (1)	O2^iv—S—O2—O1ⁱⁱ	−57.37 (4)
O2—S—O1—O3^x	−121.17 (6)	O1^iv—S—O2—O3	118.82 (6)
O2^iv—S—O1—O3^x	120.43 (6)	O1—S—O2—O3	−119.60 (6)
O1^iv—S—O1—O2^xi	−54.20 (6)	O2^iv—S—O2—O3	0.0
O2—S—O1—O2^xi	−175.37 (7)	O1^iv—S—O2—O1^xii	−47.27 (8)
O2^iv—S—O1—O2^xi	66.23 (10)	O1—S—O2—O1^xii	74.30 (6)
O1^iv—S—O1—O2^vii	−149.10 (7)	O2^iv—S—O2—O1^xii	−166.10 (6)
O2—S—O1—O2^vii	89.74 (7)	O1^iv—S—O2—O1^vii	170.83 (6)
O2^iv—S—O1—O2^vii	−28.67 (8)	O1—S—O2—O1^vii	−67.60 (7)
O1^iv—S—O2—Fe	77.73 (10)	O2^iv—S—O2—O1^vii	52.00 (3)
O1—S—O2—Fe	−160.70 (9)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x, y, −z+1/2; (v) x, −y+1, z−1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, y−1, z; (xi) x, −y, z+1/2; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.82 (2)	1.99 (2)	2.7285 (14)	148 (2)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(FeSO4H2O_He_60K) top

Crystal data top

FeH₂O₅S	Z = 4
M_r = 169.93	F(000) = 336
Monoclinic, C2/c	D_x = 3.109 Mg m⁻³
a = 7.0320 (8) Å	Mo Kα radiation, λ = 0.71073 Å
b = 7.5783 (6) Å	µ = 4.61 mm⁻¹
c = 7.7396 (8) Å	T = 60 K
β = 118.328 (14)°	0.32 × 0.29 × 0.07 mm
V = 363.06 (8) Å³

Data collection top

1189 measured reflections	θ_max = 29.4°, θ_min = 4.2°
442 independent reflections	h = −9→9
423 reflections with I > 2σ(I)	k = −9→9
R_int = 0.021	l = −10→7

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.018	w = 1/[σ²(F_o²) + (0.020P)² + 0.310P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.044	(Δ/σ)_max < 0.001
S = 1.09	Δρ_max = 0.51 e Å⁻³
442 reflections	Δρ_min = −0.44 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0330 (19)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe	0.000000	0.500000	0.000000	0.00233 (16)
S	0.000000	0.15520 (8)	0.250000	0.00232 (18)
O1	0.1684 (2)	0.04575 (18)	0.40074 (19)	0.0050 (3)
O2	0.1003 (2)	0.27048 (16)	0.15946 (17)	0.0043 (3)
O3	0.000000	0.6434 (3)	0.250000	0.0043 (4)
H	0.102 (4)	0.711 (3)	0.294 (3)	0.012 (6)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe	0.0024 (2)	0.0018 (2)	0.0024 (2)	0.00016 (13)	0.00083 (17)	0.00064 (12)
S	0.0020 (3)	0.0020 (3)	0.0030 (3)	0.000	0.0012 (2)	0.000
O1	0.0038 (7)	0.0051 (6)	0.0055 (6)	0.0007 (5)	0.0018 (5)	0.0012 (5)
O2	0.0037 (7)	0.0041 (7)	0.0056 (6)	0.0005 (5)	0.0028 (5)	0.0020 (5)
O3	0.0034 (10)	0.0044 (9)	0.0046 (9)	0.000	0.0015 (8)	0.000

Geometric parameters (Å, º) top

Fe—O2	2.0542 (12)	O1—O1^v	2.410 (3)
Fe—O2ⁱ	2.0543 (12)	O1—O2^v	2.4192 (18)
Fe—O1ⁱⁱ	2.1090 (14)	O1—O2^vi	2.8166 (18)
Fe—O1ⁱⁱⁱ	2.1090 (14)	O1—O3^vii	2.9693 (17)
Fe—O3	2.2192 (10)	O1—O2^viii	3.0663 (19)
Fe—O3ⁱ	2.2192 (10)	O1—O3^ix	3.1509 (14)
Fe—O2ⁱⁱ	3.4666 (14)	O1—O3^x	3.279 (2)
Fe—O2ⁱⁱⁱ	3.4666 (14)	O1—O2^xi	3.3002 (17)
Fe—O2^iv	3.4977 (12)	O1—O2^vii	3.3041 (18)
Fe—O2^v	3.4977 (12)	O2—O2^v	2.415 (2)
S—O1^v	1.4630 (14)	O2—O3^ix	2.7292 (15)
S—O1	1.4630 (14)	O2—O3ⁱ	2.9740 (12)
S—O2^v	1.4903 (12)	O2—O3	3.073 (2)
S—O2	1.4903 (12)	O3—H	0.81 (2)
O1—O2	2.4018 (18)	O3—H^v	0.81 (2)

O2—Fe—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	72.47 (6)
O2—Fe—O1ⁱⁱ	94.86 (5)	S—O2—O3ⁱ	134.73 (7)
O2ⁱ—Fe—O1ⁱⁱ	85.14 (5)	Fe—O2—O3ⁱ	48.23 (4)
O2—Fe—O1ⁱⁱⁱ	85.14 (5)	O1—O2—O3ⁱ	147.47 (7)
O2ⁱ—Fe—O1ⁱⁱⁱ	94.86 (5)	O2^v—O2—O3ⁱ	135.23 (8)
O1ⁱⁱ—Fe—O1ⁱⁱⁱ	180.0	O1^v—O2—O3ⁱ	100.41 (6)
O2—Fe—O3	91.88 (5)	O3^ix—O2—O3ⁱ	92.62 (4)
O2ⁱ—Fe—O3	88.12 (5)	O1ⁱⁱⁱ—O2—O3ⁱ	61.63 (4)
O1ⁱⁱ—Fe—O3	86.60 (4)	S—O2—O1ⁱⁱ	91.72 (6)
O1ⁱⁱⁱ—Fe—O3	93.40 (4)	Fe—O2—O1ⁱⁱ	43.26 (3)
O2—Fe—O3ⁱ	88.12 (5)	O1—O2—O1ⁱⁱ	126.87 (7)
O2ⁱ—Fe—O3ⁱ	91.88 (5)	O2^v—O2—O1ⁱⁱ	73.05 (6)
O1ⁱⁱ—Fe—O3ⁱ	93.40 (4)	O1^v—O2—O1ⁱⁱ	75.69 (6)
O1ⁱⁱⁱ—Fe—O3ⁱ	86.60 (4)	O3^ix—O2—O1ⁱⁱ	155.26 (5)
O3—Fe—O3ⁱ	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	91.51 (5)
O2—Fe—O2ⁱⁱ	83.08 (2)	O3ⁱ—O2—O1ⁱⁱ	62.86 (4)
O2ⁱ—Fe—O2ⁱⁱ	96.92 (2)	S—O2—O3	102.75 (6)
O1ⁱⁱ—Fe—O2ⁱⁱ	42.98 (4)	Fe—O2—O3	46.20 (3)
O1ⁱⁱⁱ—Fe—O2ⁱⁱ	137.02 (4)	O1—O2—O3	117.22 (5)
O3—Fe—O2ⁱⁱ	128.10 (3)	O2^v—O2—O3	66.87 (3)
O3ⁱ—Fe—O2ⁱⁱ	51.90 (3)	O1^v—O2—O3	116.64 (6)
O2—Fe—O2ⁱⁱⁱ	96.92 (2)	O3^ix—O2—O3	125.86 (6)
O2ⁱ—Fe—O2ⁱⁱⁱ	83.08 (2)	O1ⁱⁱⁱ—O2—O3	64.51 (4)
O1ⁱⁱ—Fe—O2ⁱⁱⁱ	137.02 (4)	O3ⁱ—O2—O3	94.42 (4)
O1ⁱⁱⁱ—Fe—O2ⁱⁱⁱ	42.98 (4)	O1ⁱⁱ—O2—O3	57.85 (3)
O3—Fe—O2ⁱⁱⁱ	51.90 (3)	S—O2—O1^xii	95.56 (6)
O3ⁱ—Fe—O2ⁱⁱⁱ	128.10 (3)	Fe—O2—O1^xii	110.96 (5)
O2ⁱⁱ—Fe—O2ⁱⁱⁱ	180.0	O1—O2—O1^xii	85.64 (4)
O2—Fe—O2^iv	137.66 (5)	O2^v—O2—O1^xii	130.17 (4)
O2ⁱ—Fe—O2^iv	42.34 (5)	O1^v—O2—O1^xii	72.35 (5)
O1ⁱⁱ—Fe—O2^iv	113.00 (4)	O3^ix—O2—O1^xii	58.09 (4)
O1ⁱⁱⁱ—Fe—O2^iv	67.00 (4)	O1ⁱⁱⁱ—O2—O1^xii	100.14 (5)
O3—Fe—O2^iv	119.80 (5)	O3ⁱ—O2—O1^xii	62.75 (5)
O3ⁱ—Fe—O2^iv	60.20 (5)	O1ⁱⁱ—O2—O1^xii	108.51 (5)
O2ⁱⁱ—Fe—O2^iv	95.84 (3)	O3—O2—O1^xii	157.10 (5)
O2ⁱⁱⁱ—Fe—O2^iv	84.16 (3)	S—O2—O1^vii	82.77 (5)
O2—Fe—O2^v	42.34 (5)	Fe—O2—O1^vii	97.06 (5)
O2ⁱ—Fe—O2^v	137.66 (5)	O1—O2—O1^vii	71.27 (6)
O1ⁱⁱ—Fe—O2^v	67.00 (4)	O2^v—O2—O1^vii	62.59 (5)
O1ⁱⁱⁱ—Fe—O2^v	113.00 (4)	O1^v—O2—O1^vii	116.92 (6)
O3—Fe—O2^v	60.20 (5)	O3^ix—O2—O1^vii	86.60 (5)
O3ⁱ—Fe—O2^v	119.80 (5)	O1ⁱⁱⁱ—O2—O1^vii	79.49 (4)
O2ⁱⁱ—Fe—O2^v	84.16 (3)	O3ⁱ—O2—O1^vii	139.21 (6)
O2ⁱⁱⁱ—Fe—O2^v	95.84 (3)	O1ⁱⁱ—O2—O1^vii	109.40 (5)
O2^iv—Fe—O2^v	180.00 (2)	O3—O2—O1^vii	55.36 (3)
O1^v—S—O1	110.92 (12)	O1^xii—O2—O1^vii	142.09 (5)
O1^v—S—O2^v	108.83 (7)	Fe—O3—Fe^v	121.36 (9)
O1—S—O2^v	110.00 (7)	Fe—O3—O2ⁱⁱⁱ	88.32 (3)
O1^v—S—O2	110.00 (7)	Fe^v—O3—O2ⁱⁱⁱ	112.02 (3)
O1—S—O2	108.83 (7)	Fe—O3—O2^xiii	112.02 (3)
O2^v—S—O2	108.22 (10)	Fe^v—O3—O2^xiii	88.32 (3)
S—O1—Fe^vi	136.08 (8)	O2ⁱⁱⁱ—O3—O2^xiii	138.67 (9)
S—O1—O2	35.97 (5)	Fe—O3—O1ⁱⁱ	45.15 (3)
Fe^vi—O1—O2	100.24 (6)	Fe^v—O3—O1ⁱⁱ	103.44 (6)
S—O1—O1^v	34.54 (6)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	132.24 (4)
Fe^vi—O1—O1^v	139.58 (9)	O2^xiii—O3—O1ⁱⁱ	70.64 (4)
O2—O1—O1^v	60.36 (5)	Fe—O3—O1^vii	103.44 (6)
S—O1—O2^v	35.37 (4)	Fe^v—O3—O1^vii	45.15 (3)
Fe^vi—O1—O2^v	144.43 (8)	O2ⁱⁱⁱ—O3—O1^vii	70.64 (4)
O2—O1—O2^v	60.12 (6)	O2^xiii—O3—O1^vii	132.24 (4)
O1^v—O1—O2^v	59.64 (5)	O1ⁱⁱ—O3—O1^vii	122.27 (9)
S—O1—O2^vi	126.90 (7)	Fe—O3—O2^xiv	159.79 (7)
Fe^vi—O1—O2^vi	46.61 (4)	Fe^v—O3—O2^xiv	43.66 (3)
O2—O1—O2^vi	108.32 (5)	O2ⁱⁱⁱ—O3—O2^xiv	87.38 (4)
O1^v—O1—O2^vi	102.66 (6)	O2^xiii—O3—O2^xiv	83.73 (4)
O2^v—O1—O2^vi	161.64 (8)	O1ⁱⁱ—O3—O2^xiv	139.70 (4)
S—O1—O3^vii	171.30 (8)	O1^vii—O3—O2^xiv	56.58 (4)
Fe^vi—O1—O3^vii	48.25 (3)	Fe—O3—O2ⁱ	43.66 (3)
O2—O1—O3^vii	146.18 (7)	Fe^v—O3—O2ⁱ	159.79 (7)
O1^v—O1—O3^vii	150.20 (5)	O2ⁱⁱⁱ—O3—O2ⁱ	83.73 (4)
O2^v—O1—O3^vii	136.00 (6)	O2^xiii—O3—O2ⁱ	87.38 (4)
O2^vi—O1—O3^vii	61.80 (4)	O1ⁱⁱ—O3—O2ⁱ	56.58 (4)
S—O1—O2^viii	116.06 (8)	O1^vii—O3—O2ⁱ	139.70 (4)
Fe^vi—O1—O2^viii	41.88 (4)	O2^xiv—O3—O2ⁱ	154.64 (9)
O2—O1—O2^viii	87.47 (5)	Fe—O3—O2	41.92 (4)
O1^v—O1—O2^viii	147.78 (5)	Fe^v—O3—O2	81.00 (6)
O2^v—O1—O2^viii	104.31 (6)	O2ⁱⁱⁱ—O3—O2	93.62 (3)
O2^vi—O1—O2^viii	88.49 (5)	O2^xiii—O3—O2	125.86 (6)
O3^vii—O1—O2^viii	61.19 (5)	O1ⁱⁱ—O3—O2	60.96 (5)
S—O1—O3^ix	91.88 (6)	O1^vii—O3—O2	66.27 (5)
Fe^vi—O1—O3^ix	44.67 (3)	O2^xiv—O3—O2	118.73 (6)
O2—O1—O3^ix	56.98 (5)	O2ⁱ—O3—O2	85.58 (4)
O1^v—O1—O3^ix	101.62 (7)	Fe—O3—O2^v	80.99 (6)
O2^v—O1—O3^ix	114.27 (6)	Fe^v—O3—O2^v	41.92 (4)
O2^vi—O1—O3^ix	61.69 (5)	O2ⁱⁱⁱ—O3—O2^v	125.86 (6)
O3^vii—O1—O3^ix	92.92 (5)	O2^xiii—O3—O2^v	93.62 (3)
O2^viii—O1—O3^ix	57.14 (4)	O1ⁱⁱ—O3—O2^v	66.27 (5)
S—O1—O3^x	102.97 (7)	O1^vii—O3—O2^v	60.96 (5)
Fe^vi—O1—O3^x	97.29 (5)	O2^xiv—O3—O2^v	85.58 (4)
O2—O1—O3^x	118.54 (6)	O2ⁱ—O3—O2^v	118.73 (6)
O1^v—O1—O3^x	68.43 (3)	O2—O3—O2^v	46.27 (5)
O2^v—O1—O3^x	117.97 (6)	Fe—O3—O1^xiii	120.93 (6)
O2^vi—O1—O3^x	52.54 (4)	Fe^v—O3—O1^xiii	41.92 (3)
O3^vii—O1—O3^x	82.53 (4)	O2ⁱⁱⁱ—O3—O1^xiii	147.21 (4)
O2^viii—O1—O3^x	137.17 (5)	O2^xiii—O3—O1^xiii	47.55 (4)
O3^ix—O1—O3^x	107.00 (5)	O1ⁱⁱ—O3—O1^xiii	79.88 (4)
S—O1—O2^xi	126.87 (8)	O1^vii—O3—O1^xiii	87.08 (5)
Fe^vi—O1—O2^xi	96.50 (5)	O2^xiv—O3—O1^xiii	60.00 (4)
O2—O1—O2^xi	162.53 (8)	O2ⁱ—O3—O1^xiii	127.09 (4)
O1^v—O1—O2^xi	103.21 (6)	O2—O3—O1^xiii	99.13 (6)
O2^v—O1—O2^xi	107.65 (5)	O2^v—O3—O1^xiii	53.79 (4)
O2^vi—O1—O2^xi	79.86 (5)	Fe—O3—O1ⁱⁱⁱ	41.92 (3)
O3^vii—O1—O2^xi	51.28 (4)	Fe^v—O3—O1ⁱⁱⁱ	120.93 (6)
O2^viii—O1—O2^xi	108.51 (5)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	47.55 (4)
O3^ix—O1—O2^xi	137.83 (6)	O2^xiii—O3—O1ⁱⁱⁱ	147.21 (4)
O3^x—O1—O2^xi	53.75 (3)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	87.08 (5)
S—O1—O2^vii	113.52 (7)	O1^vii—O3—O1ⁱⁱⁱ	79.88 (4)
Fe^vi—O1—O2^vii	77.02 (5)	O2^xiv—O3—O1ⁱⁱⁱ	127.09 (4)
O2—O1—O2^vii	108.73 (5)	O2ⁱ—O3—O1ⁱⁱⁱ	60.00 (4)
O1^v—O1—O2^vii	140.76 (7)	O2—O3—O1ⁱⁱⁱ	53.79 (4)
O2^v—O1—O2^vii	81.91 (4)	O2^v—O3—O1ⁱⁱⁱ	99.13 (6)
O2^vi—O1—O2^vii	116.23 (6)	O1^xiii—O3—O1ⁱⁱⁱ	152.83 (8)
O3^vii—O1—O2^vii	58.37 (5)	Fe—O3—H	107.7 (16)
O2^viii—O1—O2^vii	44.36 (5)	Fe^v—O3—H	108.1 (16)
O3^ix—O1—O2^vii	101.16 (5)	O2ⁱⁱⁱ—O3—H	21.8 (17)
O3^x—O1—O2^vii	132.59 (5)	O2^xiii—O3—H	119.1 (18)
O2^xi—O1—O2^vii	79.82 (3)	O1ⁱⁱ—O3—H	147.0 (16)
S—O2—Fe	132.42 (8)	O1^vii—O3—H	76.4 (17)
S—O2—O1	35.21 (5)	O2^xiv—O3—H	72.8 (16)
Fe—O2—O1	162.26 (7)	O2ⁱ—O3—H	91.2 (16)
S—O2—O2^v	35.89 (5)	O2—O3—H	114.7 (17)
Fe—O2—O2^v	102.71 (5)	O2^v—O3—H	137.3 (17)
O1—O2—O2^v	60.30 (5)	O1^xiii—O3—H	131.1 (16)
S—O2—O1^v	34.63 (4)	O1ⁱⁱⁱ—O3—H	68.7 (17)
Fe—O2—O1^v	117.79 (7)	Fe—O3—H^v	108.1 (16)
O1—O2—O1^v	59.99 (7)	Fe^v—O3—H^v	107.7 (16)
O2^v—O2—O1^v	59.58 (5)	O2ⁱⁱⁱ—O3—H^v	119.1 (18)
S—O2—O3^ix	109.39 (7)	O2^xiii—O3—H^v	21.8 (17)
Fe—O2—O3^ix	118.12 (6)	O1ⁱⁱ—O3—H^v	76.4 (17)
O1—O2—O3^ix	75.47 (5)	O1^vii—O3—H^v	147.0 (16)
O2^v—O2—O3^ix	131.69 (7)	O2^xiv—O3—H^v	91.2 (16)
O1^v—O2—O3^ix	114.59 (7)	O2ⁱ—O3—H^v	72.8 (16)
S—O2—O1ⁱⁱⁱ	162.04 (8)	O2—O3—H^v	137.3 (17)
Fe—O2—O1ⁱⁱⁱ	48.25 (4)	O2^v—O3—H^v	114.7 (17)
O1—O2—O1ⁱⁱⁱ	137.40 (6)	O1^xiii—O3—H^v	68.7 (17)
O2^v—O2—O1ⁱⁱⁱ	129.66 (4)	O1ⁱⁱⁱ—O3—H^v	131.1 (16)
O1^v—O2—O1ⁱⁱⁱ	161.64 (8)	H—O3—H^v	102 (3)

O1^v—S—O1—Fe^vi	115.28 (12)	O2^v—S—O2—Fe	−41.01 (7)
O2^v—S—O1—Fe^vi	−124.27 (11)	O1^v—S—O2—O1	−121.71 (11)
O2—S—O1—Fe^vi	−5.86 (14)	O2^v—S—O2—O1	119.52 (7)
O1^v—S—O1—O2	121.14 (6)	O1^v—S—O2—O2^v	118.78 (7)
O2^v—S—O1—O2	−118.41 (10)	O1—S—O2—O2^v	−119.52 (7)
O2^v—S—O1—O1^v	120.45 (6)	O1—S—O2—O1^v	121.71 (11)
O2—S—O1—O1^v	−121.14 (6)	O2^v—S—O2—O1^v	−118.78 (7)
O1^v—S—O1—O2^v	−120.45 (6)	O1^v—S—O2—O3^ix	−105.47 (8)
O2—S—O1—O2^v	118.41 (10)	O1—S—O2—O3^ix	16.24 (9)
O1^v—S—O1—O2^vi	52.59 (7)	O2^v—S—O2—O3^ix	135.76 (8)
O2^v—S—O1—O2^vi	173.04 (10)	O1^v—S—O2—O1ⁱⁱⁱ	161.7 (3)
O2—S—O1—O2^vi	−68.56 (10)	O1—S—O2—O1ⁱⁱⁱ	−76.6 (3)
O1^v—S—O1—O2^viii	161.89 (9)	O2^v—S—O2—O1ⁱⁱⁱ	42.9 (2)
O2^v—S—O1—O2^viii	−77.66 (9)	O1^v—S—O2—O3ⁱ	9.17 (13)
O2—S—O1—O2^viii	40.74 (8)	O1—S—O2—O3ⁱ	130.88 (10)
O1^v—S—O1—O3^ix	107.93 (6)	O2^v—S—O2—O3ⁱ	−109.61 (11)
O2^v—S—O1—O3^ix	−131.62 (7)	O1^v—S—O2—O1ⁱⁱ	61.40 (8)
O2—S—O1—O3^ix	−13.22 (7)	O1—S—O2—O1ⁱⁱ	−176.90 (6)
O1^v—S—O1—O3^x	0.0	O2^v—S—O2—O1ⁱⁱ	−57.38 (4)
O2^v—S—O1—O3^x	120.45 (6)	O1^v—S—O2—O3	118.78 (7)
O2—S—O1—O3^x	−121.14 (6)	O1—S—O2—O3	−119.52 (7)
O1^v—S—O1—O2^xi	−54.15 (6)	O2^v—S—O2—O3	0.0
O2^v—S—O1—O2^xi	66.30 (11)	O1^v—S—O2—O1^xii	−47.39 (9)
O2—S—O1—O2^xi	−175.29 (8)	O1—S—O2—O1^xii	74.31 (6)
O1^v—S—O1—O2^vii	−149.05 (8)	O2^v—S—O2—O1^xii	−166.17 (7)
O2^v—S—O1—O2^vii	−28.60 (9)	O1^v—S—O2—O1^vii	170.73 (7)
O2—S—O1—O2^vii	89.81 (7)	O1—S—O2—O1^vii	−67.56 (8)
O1^v—S—O2—Fe	77.76 (11)	O2^v—S—O2—O1^vii	51.96 (4)
O1—S—O2—Fe	−160.53 (9)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x, −y+1, z−1/2; (v) −x, y, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, y−1, z; (xi) x, −y, z+1/2; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.81 (2)	2.00 (2)	2.7292 (15)	150 (2)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(FeSO4H2O_He_75K) top

Crystal data top

FeH₂O₅S	Z = 4
M_r = 169.93	F(000) = 336
Monoclinic, C2/c	D_x = 3.107 Mg m⁻³
a = 7.0337 (9) Å	Mo Kα radiation, λ = 0.71073 Å
b = 7.5789 (7) Å	µ = 4.61 mm⁻¹
c = 7.7406 (9) Å	T = 75 K
β = 118.325 (16)°	0.32 × 0.29 × 0.07 mm
V = 363.23 (9) Å³

Data collection top

1202 measured reflections	θ_max = 29.4°, θ_min = 4.2°
445 independent reflections	h = −9→9
425 reflections with I > 2σ(I)	k = −9→9
R_int = 0.019	l = −10→7

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.019	w = 1/[σ²(F_o²) + (0.029P)² + 0.140P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.052	(Δ/σ)_max < 0.001
S = 1.12	Δρ_max = 0.62 e Å⁻³
445 reflections	Δρ_min = −0.55 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.035 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe	0.000000	0.500000	0.000000	0.00280 (18)
S	0.000000	0.15532 (8)	0.250000	0.0027 (2)
O1	0.1686 (2)	0.0458 (2)	0.40091 (19)	0.0052 (3)
O2	0.1002 (2)	0.27064 (17)	0.15934 (18)	0.0049 (3)
O3	0.000000	0.6434 (3)	0.250000	0.0046 (4)
H	0.098 (4)	0.712 (3)	0.291 (3)	0.011 (6)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe	0.0025 (3)	0.0027 (3)	0.0028 (2)	0.00005 (13)	0.00097 (18)	0.00058 (12)
S	0.0021 (4)	0.0026 (3)	0.0030 (3)	0.000	0.0010 (3)	0.000
O1	0.0039 (7)	0.0047 (7)	0.0060 (6)	0.0012 (6)	0.0016 (5)	0.0018 (5)
O2	0.0041 (7)	0.0047 (7)	0.0062 (6)	0.0005 (5)	0.0027 (5)	0.0020 (5)
O3	0.0039 (10)	0.0050 (10)	0.0046 (9)	0.000	0.0017 (8)	0.000

Geometric parameters (Å, º) top

Fe—O2	2.0530 (13)	O1—O1^v	2.414 (3)
Fe—O2ⁱ	2.0530 (13)	O1—O2^v	2.4204 (19)
Fe—O1ⁱⁱ	2.1085 (15)	O1—O2^vi	2.8163 (19)
Fe—O1ⁱⁱⁱ	2.1085 (15)	O1—O3^vii	2.9691 (18)
Fe—O3	2.2195 (10)	O1—O2^viii	3.064 (2)
Fe—O3ⁱ	2.2195 (10)	O1—O3^ix	3.1510 (15)
Fe—O2ⁱⁱ	3.4686 (14)	O1—O3^x	3.280 (2)
Fe—O2ⁱⁱⁱ	3.4686 (14)	O1—O2^xi	3.3014 (18)
Fe—O2^iv	3.4979 (13)	O1—O2^vii	3.3035 (19)
Fe—O2^v	3.4979 (13)	O2—O2^v	2.415 (2)
S—O1^v	1.4645 (15)	O2—O3^ix	2.7307 (15)
S—O1	1.4645 (15)	O2—O3ⁱ	2.9735 (13)
S—O2	1.4908 (13)	O2—O3	3.073 (2)
S—O2^v	1.4908 (13)	O3—H	0.80 (3)
O1—O2	2.4036 (19)	O3—H^v	0.80 (2)

O2—Fe—O2ⁱ	180.00 (8)	O3^ix—O2—O1ⁱⁱⁱ	72.48 (6)
O2—Fe—O1ⁱⁱ	94.83 (5)	S—O2—O3ⁱ	134.75 (7)
O2ⁱ—Fe—O1ⁱⁱ	85.17 (5)	Fe—O2—O3ⁱ	48.25 (4)
O2—Fe—O1ⁱⁱⁱ	85.17 (5)	O1—O2—O3ⁱ	147.46 (8)
O2ⁱ—Fe—O1ⁱⁱⁱ	94.83 (5)	O2^v—O2—O3ⁱ	135.28 (8)
O1ⁱⁱ—Fe—O1ⁱⁱⁱ	180.0	O1^v—O2—O3ⁱ	100.39 (6)
O2—Fe—O3	91.88 (5)	O3^ix—O2—O3ⁱ	92.62 (5)
O2ⁱ—Fe—O3	88.12 (5)	O1ⁱⁱⁱ—O2—O3ⁱ	61.63 (5)
O1ⁱⁱ—Fe—O3	86.59 (4)	S—O2—O1ⁱⁱ	91.73 (7)
O1ⁱⁱⁱ—Fe—O3	93.41 (4)	Fe—O2—O1ⁱⁱ	43.29 (4)
O2—Fe—O3ⁱ	88.12 (5)	O1—O2—O1ⁱⁱ	126.89 (8)
O2ⁱ—Fe—O3ⁱ	91.88 (5)	O2^v—O2—O1ⁱⁱ	73.07 (6)
O1ⁱⁱ—Fe—O3ⁱ	93.41 (4)	O1^v—O2—O1ⁱⁱ	75.66 (6)
O1ⁱⁱⁱ—Fe—O3ⁱ	86.59 (4)	O3^ix—O2—O1ⁱⁱ	155.29 (6)
O3—Fe—O3ⁱ	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	91.53 (5)
O2—Fe—O2ⁱⁱ	83.07 (2)	O3ⁱ—O2—O1ⁱⁱ	62.90 (4)
O2ⁱ—Fe—O2ⁱⁱ	96.93 (2)	S—O2—O3	102.75 (6)
O1ⁱⁱ—Fe—O2ⁱⁱ	42.99 (4)	Fe—O2—O3	46.22 (3)
O1ⁱⁱⁱ—Fe—O2ⁱⁱ	137.01 (4)	O1—O2—O3	117.20 (6)
O3—Fe—O2ⁱⁱ	128.10 (3)	O2^v—O2—O3	66.86 (3)
O3ⁱ—Fe—O2ⁱⁱ	51.90 (3)	O1^v—O2—O3	116.64 (6)
O2—Fe—O2ⁱⁱⁱ	96.93 (2)	O3^ix—O2—O3	125.86 (6)
O2ⁱ—Fe—O2ⁱⁱⁱ	83.07 (2)	O1ⁱⁱⁱ—O2—O3	64.53 (4)
O1ⁱⁱ—Fe—O2ⁱⁱⁱ	137.01 (4)	O3ⁱ—O2—O3	94.47 (4)
O1ⁱⁱⁱ—Fe—O2ⁱⁱⁱ	42.99 (4)	O1ⁱⁱ—O2—O3	57.87 (4)
O3—Fe—O2ⁱⁱⁱ	51.90 (3)	S—O2—O1^xii	95.55 (6)
O3ⁱ—Fe—O2ⁱⁱⁱ	128.10 (3)	Fe—O2—O1^xii	111.00 (5)
O2ⁱⁱ—Fe—O2ⁱⁱⁱ	180.0	O1—O2—O1^xii	85.61 (4)
O2—Fe—O2^iv	137.66 (5)	O2^v—O2—O1^xii	130.17 (4)
O2ⁱ—Fe—O2^iv	42.34 (5)	O1^v—O2—O1^xii	72.36 (6)
O1ⁱⁱ—Fe—O2^iv	113.02 (5)	O3^ix—O2—O1^xii	58.05 (4)
O1ⁱⁱⁱ—Fe—O2^iv	66.98 (5)	O1ⁱⁱⁱ—O2—O1^xii	100.14 (5)
O3—Fe—O2^iv	119.82 (5)	O3ⁱ—O2—O1^xii	62.77 (5)
O3ⁱ—Fe—O2^iv	60.18 (5)	O1ⁱⁱ—O2—O1^xii	108.56 (5)
O2ⁱⁱ—Fe—O2^iv	95.82 (3)	O3—O2—O1^xii	157.16 (5)
O2ⁱⁱⁱ—Fe—O2^iv	84.18 (3)	S—O2—O1^vii	82.72 (6)
O2—Fe—O2^v	42.34 (5)	Fe—O2—O1^vii	97.09 (5)
O2ⁱ—Fe—O2^v	137.66 (5)	O1—O2—O1^vii	71.21 (6)
O1ⁱⁱ—Fe—O2^v	66.98 (5)	O2^v—O2—O1^vii	62.55 (5)
O1ⁱⁱⁱ—Fe—O2^v	113.02 (5)	O1^v—O2—O1^vii	116.91 (6)
O3—Fe—O2^v	60.18 (5)	O3^ix—O2—O1^vii	86.58 (5)
O3ⁱ—Fe—O2^v	119.82 (5)	O1ⁱⁱⁱ—O2—O1^vii	79.53 (4)
O2ⁱⁱ—Fe—O2^v	84.18 (3)	O3ⁱ—O2—O1^vii	139.26 (6)
O2ⁱⁱⁱ—Fe—O2^v	95.82 (3)	O1ⁱⁱ—O2—O1^vii	109.42 (6)
O2^iv—Fe—O2^v	180.00 (2)	O3—O2—O1^vii	55.36 (3)
O1^v—S—O1	110.98 (12)	O1^xii—O2—O1^vii	142.02 (5)
O1^v—S—O2	109.96 (7)	Fe—O3—Fe^v	121.35 (9)
O1—S—O2	108.84 (8)	Fe—O3—O2^xiii	112.01 (3)
O1^v—S—O2^v	108.84 (8)	Fe^v—O3—O2^xiii	88.34 (3)
O1—S—O2^v	109.96 (7)	Fe—O3—O2ⁱⁱⁱ	88.34 (3)
O2—S—O2^v	108.21 (11)	Fe^v—O3—O2ⁱⁱⁱ	112.02 (3)
S—O1—Fe^vi	136.10 (8)	O2^xiii—O3—O2ⁱⁱⁱ	138.65 (10)
S—O1—O2	35.95 (5)	Fe—O3—O1ⁱⁱ	45.15 (3)
Fe^vi—O1—O2	100.28 (6)	Fe^v—O3—O1ⁱⁱ	103.42 (6)
S—O1—O1^v	34.51 (6)	O2^xiii—O3—O1ⁱⁱ	70.65 (4)
Fe^vi—O1—O1^v	139.56 (9)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	132.26 (4)
O2—O1—O1^v	60.32 (5)	Fe—O3—O1^vii	103.42 (6)
S—O1—O2^v	35.37 (5)	Fe^v—O3—O1^vii	45.15 (3)
Fe^vi—O1—O2^v	144.46 (8)	O2^xiii—O3—O1^vii	132.26 (4)
O2—O1—O2^v	60.09 (7)	O2ⁱⁱⁱ—O3—O1^vii	70.65 (4)
O1^v—O1—O2^v	59.63 (5)	O1ⁱⁱ—O3—O1^vii	122.22 (9)
S—O1—O2^vi	126.88 (8)	Fe—O3—O2^xiv	159.77 (7)
Fe^vi—O1—O2^vi	46.58 (4)	Fe^v—O3—O2^xiv	43.64 (3)
O2—O1—O2^vi	108.32 (5)	O2^xiii—O3—O2^xiv	83.74 (4)
O1^v—O1—O2^vi	102.66 (6)	O2ⁱⁱⁱ—O3—O2^xiv	87.38 (5)
O2^v—O1—O2^vi	161.63 (8)	O1ⁱⁱ—O3—O2^xiv	139.68 (5)
S—O1—O3^vii	171.33 (8)	O1^vii—O3—O2^xiv	56.58 (4)
Fe^vi—O1—O3^vii	48.26 (3)	Fe—O3—O2ⁱ	43.64 (3)
O2—O1—O3^vii	146.24 (7)	Fe^v—O3—O2ⁱ	159.77 (7)
O1^v—O1—O3^vii	150.17 (5)	O2^xiii—O3—O2ⁱ	87.38 (5)
O2^v—O1—O3^vii	136.02 (6)	O2ⁱⁱⁱ—O3—O2ⁱ	83.74 (4)
O2^vi—O1—O3^vii	61.79 (4)	O1ⁱⁱ—O3—O2ⁱ	56.58 (4)
S—O1—O2^viii	116.10 (8)	O1^vii—O3—O2ⁱ	139.68 (5)
Fe^vi—O1—O2^viii	41.88 (4)	O2^xiv—O3—O2ⁱ	154.69 (9)
O2—O1—O2^viii	87.52 (5)	Fe—O3—O2	41.90 (4)
O1^v—O1—O2^viii	147.79 (5)	Fe^v—O3—O2	81.01 (6)
O2^v—O1—O2^viii	104.34 (6)	O2^xiii—O3—O2	125.86 (6)
O2^vi—O1—O2^viii	88.47 (5)	O2ⁱⁱⁱ—O3—O2	93.64 (4)
O3^vii—O1—O2^viii	61.21 (5)	O1ⁱⁱ—O3—O2	60.92 (5)
S—O1—O3^ix	91.88 (6)	O1^vii—O3—O2	66.27 (5)
Fe^vi—O1—O3^ix	44.68 (3)	O2^xiv—O3—O2	118.73 (6)
O2—O1—O3^ix	57.00 (5)	O2ⁱ—O3—O2	85.53 (4)
O1^v—O1—O3^ix	101.61 (7)	Fe—O3—O2^v	81.01 (6)
O2^v—O1—O3^ix	114.26 (7)	Fe^v—O3—O2^v	41.90 (4)
O2^vi—O1—O3^ix	61.68 (5)	O2^xiii—O3—O2^v	93.64 (4)
O3^vii—O1—O3^ix	92.94 (5)	O2ⁱⁱⁱ—O3—O2^v	125.86 (6)
O2^viii—O1—O3^ix	57.14 (4)	O1ⁱⁱ—O3—O2^v	66.27 (5)
S—O1—O3^x	102.92 (7)	O1^vii—O3—O2^v	60.92 (5)
Fe^vi—O1—O3^x	97.29 (5)	O2^xiv—O3—O2^v	85.53 (4)
O2—O1—O3^x	118.49 (6)	O2ⁱ—O3—O2^v	118.73 (6)
O1^v—O1—O3^x	68.41 (3)	O2—O3—O2^v	46.29 (6)
O2^v—O1—O3^x	117.94 (6)	Fe—O3—O1^xiii	120.95 (6)
O2^vi—O1—O3^x	52.56 (4)	Fe^v—O3—O1^xiii	41.91 (3)
O3^vii—O1—O3^x	82.53 (4)	O2^xiii—O3—O1^xiii	47.58 (4)
O2^viii—O1—O3^x	137.17 (6)	O2ⁱⁱⁱ—O3—O1^xiii	147.17 (4)
O3^ix—O1—O3^x	106.99 (5)	O1ⁱⁱ—O3—O1^xiii	79.90 (4)
S—O1—O2^xi	126.82 (8)	O1^vii—O3—O1^xiii	87.06 (5)
Fe^vi—O1—O2^xi	96.53 (5)	O2^xiv—O3—O1^xiii	59.96 (4)
O2—O1—O2^xi	162.45 (8)	O2ⁱ—O3—O1^xiii	127.12 (4)
O1^v—O1—O2^xi	103.17 (6)	O2—O3—O1^xiii	99.15 (6)
O2^v—O1—O2^xi	107.64 (6)	O2^v—O3—O1^xiii	53.79 (4)
O2^vi—O1—O2^xi	79.86 (5)	Fe—O3—O1ⁱⁱⁱ	41.91 (3)
O3^vii—O1—O2^xi	51.30 (4)	Fe^v—O3—O1ⁱⁱⁱ	120.95 (6)
O2^viii—O1—O2^xi	108.56 (5)	O2^xiii—O3—O1ⁱⁱⁱ	147.17 (4)
O3^ix—O1—O2^xi	137.84 (6)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	47.58 (4)
O3^x—O1—O2^xi	53.72 (3)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	87.06 (5)
S—O1—O2^vii	113.56 (8)	O1^vii—O3—O1ⁱⁱⁱ	79.90 (4)
Fe^vi—O1—O2^vii	77.04 (5)	O2^xiv—O3—O1ⁱⁱⁱ	127.12 (4)
O2—O1—O2^vii	108.79 (6)	O2ⁱ—O3—O1ⁱⁱⁱ	59.96 (4)
O1^v—O1—O2^vii	140.77 (7)	O2—O3—O1ⁱⁱⁱ	53.79 (4)
O2^v—O1—O2^vii	81.94 (5)	O2^v—O3—O1ⁱⁱⁱ	99.15 (6)
O2^vi—O1—O2^vii	116.22 (6)	O1^xiii—O3—O1ⁱⁱⁱ	152.85 (9)
O3^vii—O1—O2^vii	58.37 (5)	Fe—O3—H	107.8 (17)
O2^viii—O1—O2^vii	44.39 (5)	Fe^v—O3—H	109.5 (17)
O3^ix—O1—O2^vii	101.19 (5)	O2^xiii—O3—H	117.4 (18)
O3^x—O1—O2^vii	132.57 (5)	O2ⁱⁱⁱ—O3—H	22.9 (18)
O2^xi—O1—O2^vii	79.84 (3)	O1ⁱⁱ—O3—H	146.1 (17)
S—O2—Fe	132.45 (8)	O1^vii—O3—H	78.5 (17)
S—O2—O1	35.22 (5)	O2^xiv—O3—H	73.4 (17)
Fe—O2—O1	162.27 (7)	O2ⁱ—O3—H	90.0 (17)
S—O2—O2^v	35.89 (5)	O2—O3—H	116.2 (18)
Fe—O2—O2^v	102.74 (5)	O2^v—O3—H	139.3 (17)
O1—O2—O2^v	60.30 (5)	O1^xiii—O3—H	131.2 (17)
S—O2—O1^v	34.66 (4)	O1ⁱⁱⁱ—O3—H	69.4 (17)
Fe—O2—O1^v	117.78 (7)	Fe—O3—H^v	109.5 (17)
O1—O2—O1^v	60.04 (7)	Fe^v—O3—H^v	107.8 (17)
O2^v—O2—O1^v	59.61 (5)	O2^xiii—O3—H^v	22.9 (18)
S—O2—O3^ix	109.34 (7)	O2ⁱⁱⁱ—O3—H^v	117.4 (18)
Fe—O2—O3^ix	118.13 (6)	O1ⁱⁱ—O3—H^v	78.5 (17)
O1—O2—O3^ix	75.42 (6)	O1^vii—O3—H^v	146.1 (17)
O2^v—O2—O3^ix	131.64 (7)	O2^xiv—O3—H^v	90.0 (17)
O1^v—O2—O3^ix	114.58 (7)	O2ⁱ—O3—H^v	73.4 (17)
S—O2—O1ⁱⁱⁱ	162.03 (8)	O2—O3—H^v	139.3 (17)
Fe—O2—O1ⁱⁱⁱ	48.25 (4)	O2^v—O3—H^v	116.2 (18)
O1—O2—O1ⁱⁱⁱ	137.36 (6)	O1^xiii—O3—H^v	69.4 (17)
O2^v—O2—O1ⁱⁱⁱ	129.66 (4)	O1ⁱⁱⁱ—O3—H^v	131.2 (17)
O1^v—O2—O1ⁱⁱⁱ	161.63 (8)	H—O3—H^v	99 (4)

O1^v—S—O1—Fe^vi	115.22 (13)	O2^v—S—O2—Fe	−41.02 (7)
O2—S—O1—Fe^vi	−5.92 (15)	O1^v—S—O2—O1	−121.76 (12)
O2^v—S—O1—Fe^vi	−124.30 (12)	O2^v—S—O2—O1	119.48 (7)
O1^v—S—O1—O2	121.14 (6)	O1^v—S—O2—O2^v	118.76 (7)
O2^v—S—O1—O2	−118.38 (11)	O1—S—O2—O2^v	−119.48 (7)
O2—S—O1—O1^v	−121.14 (6)	O1—S—O2—O1^v	121.76 (12)
O2^v—S—O1—O1^v	120.48 (7)	O2^v—S—O2—O1^v	−118.76 (7)
O1^v—S—O1—O2^v	−120.48 (7)	O1^v—S—O2—O3^ix	−105.51 (8)
O2—S—O1—O2^v	118.38 (11)	O1—S—O2—O3^ix	16.24 (9)
O1^v—S—O1—O2^vi	52.58 (8)	O2^v—S—O2—O3^ix	135.72 (8)
O2—S—O1—O2^vi	−68.56 (11)	O1^v—S—O2—O1ⁱⁱⁱ	161.7 (3)
O2^v—S—O1—O2^vi	173.05 (11)	O1—S—O2—O1ⁱⁱⁱ	−76.5 (3)
O1^v—S—O1—O2^viii	161.87 (9)	O2^v—S—O2—O1ⁱⁱⁱ	43.0 (2)
O2—S—O1—O2^viii	40.72 (9)	O1^v—S—O2—O3ⁱ	9.08 (13)
O2^v—S—O1—O2^viii	−77.66 (9)	O1—S—O2—O3ⁱ	130.84 (11)
O1^v—S—O1—O3^ix	107.91 (6)	O2^v—S—O2—O3ⁱ	−109.68 (12)
O2—S—O1—O3^ix	−13.23 (8)	O1^v—S—O2—O1ⁱⁱ	61.36 (9)
O2^v—S—O1—O3^ix	−131.61 (7)	O1—S—O2—O1ⁱⁱ	−176.88 (7)
O1^v—S—O1—O3^x	0.0	O2^v—S—O2—O1ⁱⁱ	−57.40 (4)
O2—S—O1—O3^x	−121.14 (6)	O1^v—S—O2—O3	118.76 (7)
O2^v—S—O1—O3^x	120.48 (7)	O1—S—O2—O3	−119.48 (7)
O1^v—S—O1—O2^xi	−54.08 (7)	O2^v—S—O2—O3	0.0
O2—S—O1—O2^xi	−175.22 (8)	O1^v—S—O2—O1^xii	−47.48 (9)
O2^v—S—O1—O2^xi	66.39 (11)	O1—S—O2—O1^xii	74.28 (7)
O1^v—S—O1—O2^vii	−149.02 (8)	O2^v—S—O2—O1^xii	−166.24 (7)
O2—S—O1—O2^vii	89.84 (8)	O1^v—S—O2—O1^vii	170.71 (7)
O2^v—S—O1—O2^vii	−28.54 (9)	O1—S—O2—O1^vii	−67.53 (8)
O1^v—S—O2—Fe	77.75 (12)	O2^v—S—O2—O1^vii	51.95 (4)
O1—S—O2—Fe	−160.49 (10)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.80 (3)	2.02 (2)	2.7307 (15)	148 (2)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(FeSO4H2O_N2_113K) top

Crystal data top

FeH₂Mg₀O₅S	V = 363.48 (9) Å³
M_r = 169.93	Z = 4
Monoclinic, C2/c	F(000) = 336
a = 7.0404 (10) Å	D_x = 3.105 Mg m⁻³
b = 7.5756 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.745 (1) Å	µ = 4.61 mm⁻¹
β = 118.368 (10)°	T = 113 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.023
T_min = 0.581, T_max = 0.748	θ_max = 40.0°, θ_min = 4.2°
10314 measured reflections	h = −12→12
1128 independent reflections	k = −13→13
1118 reflections with I > 2σ(I)	l = −14→14

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.013	w = 1/[σ²(F_o²) + (0.013P)² + 0.240P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.032	(Δ/σ)_max < 0.001
S = 1.19	Δρ_max = 0.68 e Å⁻³
1128 reflections	Δρ_min = −0.44 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0419 (14)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe	0.000000	0.500000	0.000000	0.00387 (4)
S	0.000000	0.15512 (2)	0.250000	0.00351 (4)
O1	0.16853 (7)	0.04497 (6)	0.40047 (7)	0.00700 (7)
O2	0.09991 (7)	0.27015 (6)	0.15910 (6)	0.00624 (7)
O3	0.000000	0.64381 (8)	0.250000	0.00616 (9)
H	0.109 (2)	0.712 (2)	0.292 (2)	0.021 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe	0.00364 (5)	0.00378 (5)	0.00416 (5)	0.00003 (3)	0.00182 (4)	0.00046 (3)
S	0.00283 (7)	0.00326 (7)	0.00436 (7)	0.000	0.00162 (5)	0.000
O1	0.00455 (14)	0.00773 (16)	0.00792 (15)	0.00210 (12)	0.00231 (12)	0.00347 (12)
O2	0.00607 (15)	0.00564 (15)	0.00832 (15)	0.00030 (11)	0.00450 (13)	0.00221 (12)
O3	0.0060 (2)	0.0064 (2)	0.0064 (2)	0.000	0.00316 (17)	0.000

Geometric parameters (Å, º) top

Fe—O2	2.0546 (5)	O1—O1^v	2.4099 (10)
Fe—O2ⁱ	2.0546 (5)	O1—O2^v	2.4220 (7)
Fe—O1ⁱⁱ	2.1088 (5)	O1—O2^vi	2.8142 (7)
Fe—O1ⁱⁱⁱ	2.1088 (5)	O1—O3^vii	2.9693 (7)
Fe—O3ⁱ	2.2217 (4)	O1—O2^viii	3.0687 (8)
Fe—O3	2.2217 (4)	O1—O3^ix	3.1542 (6)
Fe—O2ⁱⁱ	3.4679 (6)	O1—O3^x	3.2692 (8)
Fe—O2ⁱⁱⁱ	3.4679 (6)	O1—O2^xi	3.2961 (7)
Fe—O2^iv	3.5018 (6)	O1—O2^vii	3.3122 (8)
Fe—O2^v	3.5018 (6)	O2—O2^v	2.4174 (9)
S—O1^v	1.4657 (5)	O2—O3^ix	2.7316 (6)
S—O1	1.4657 (5)	O2—O3ⁱ	2.9734 (6)
S—O2	1.4901 (5)	O2—O3	3.0780 (8)
S—O2^v	1.4901 (4)	O3—H	0.850 (15)
O1—O2	2.4041 (7)	O3—H^v	0.850 (15)

O2—Fe—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	72.23 (2)
O2—Fe—O1ⁱⁱ	94.955 (19)	S—O2—O3ⁱ	134.90 (3)
O2ⁱ—Fe—O1ⁱⁱ	85.045 (19)	Fe—O2—O3ⁱ	48.309 (15)
O2—Fe—O1ⁱⁱⁱ	85.045 (19)	O1—O2—O3ⁱ	147.41 (3)
O2ⁱ—Fe—O1ⁱⁱⁱ	94.955 (19)	O2^v—O2—O3ⁱ	135.41 (3)
O1ⁱⁱ—Fe—O1ⁱⁱⁱ	180.0	O1^v—O2—O3ⁱ	100.56 (2)
O2—Fe—O3ⁱ	88.01 (2)	O3^ix—O2—O3ⁱ	92.541 (17)
O2ⁱ—Fe—O3ⁱ	91.99 (2)	O1ⁱⁱⁱ—O2—O3ⁱ	61.660 (16)
O1ⁱⁱ—Fe—O3ⁱ	93.465 (16)	S—O2—O1ⁱⁱ	91.85 (2)
O1ⁱⁱⁱ—Fe—O3ⁱ	86.535 (16)	Fe—O2—O1ⁱⁱ	43.206 (12)
O2—Fe—O3	91.99 (2)	O1—O2—O1ⁱⁱ	127.04 (2)
O2ⁱ—Fe—O3	88.01 (2)	O2^v—O2—O1ⁱⁱ	73.19 (2)
O1ⁱⁱ—Fe—O3	86.535 (16)	O1^v—O2—O1ⁱⁱ	75.90 (2)
O1ⁱⁱⁱ—Fe—O3	93.465 (16)	O3^ix—O2—O1ⁱⁱ	155.19 (2)
O3ⁱ—Fe—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	91.50 (2)
O2—Fe—O2ⁱⁱ	83.065 (13)	O3ⁱ—O2—O1ⁱⁱ	62.915 (16)
O2ⁱ—Fe—O2ⁱⁱ	96.935 (13)	S—O2—O3	102.67 (2)
O1ⁱⁱ—Fe—O2ⁱⁱ	43.018 (15)	Fe—O2—O3	46.168 (12)
O1ⁱⁱⁱ—Fe—O2ⁱⁱ	136.982 (15)	O1—O2—O3	117.26 (2)
O3ⁱ—Fe—O2ⁱⁱ	51.934 (12)	O2^v—O2—O3	66.877 (10)
O3—Fe—O2ⁱⁱ	128.066 (12)	O1^v—O2—O3	116.67 (2)
O2—Fe—O2ⁱⁱⁱ	96.935 (13)	O3^ix—O2—O3	125.66 (2)
O2ⁱ—Fe—O2ⁱⁱⁱ	83.065 (13)	O1ⁱⁱⁱ—O2—O3	64.550 (16)
O1ⁱⁱ—Fe—O2ⁱⁱⁱ	136.982 (15)	O3ⁱ—O2—O3	94.477 (15)
O1ⁱⁱⁱ—Fe—O2ⁱⁱⁱ	43.018 (15)	O1ⁱⁱ—O2—O3	57.772 (13)
O3ⁱ—Fe—O2ⁱⁱⁱ	128.066 (12)	S—O2—O1^xii	95.85 (2)
O3—Fe—O2ⁱⁱⁱ	51.934 (12)	Fe—O2—O1^xii	110.89 (2)
O2ⁱⁱ—Fe—O2ⁱⁱⁱ	180.000 (15)	O1—O2—O1^xii	85.717 (17)
O2—Fe—O2^iv	137.682 (17)	O2^v—O2—O1^xii	130.379 (14)
O2ⁱ—Fe—O2^iv	42.319 (17)	O1^v—O2—O1^xii	72.57 (2)
O1ⁱⁱ—Fe—O2^iv	112.866 (18)	O3^ix—O2—O1^xii	58.124 (16)
O1ⁱⁱⁱ—Fe—O2^iv	67.134 (18)	O1ⁱⁱⁱ—O2—O1^xii	99.938 (19)
O3ⁱ—Fe—O2^iv	60.234 (18)	O3ⁱ—O2—O1^xii	62.610 (18)
O3—Fe—O2^iv	119.765 (18)	O1ⁱⁱ—O2—O1^xii	108.62 (2)
O2ⁱⁱ—Fe—O2^iv	95.790 (15)	O3—O2—O1^xii	156.998 (18)
O2ⁱⁱⁱ—Fe—O2^iv	84.210 (15)	S—O2—O1^vii	82.68 (2)
O2—Fe—O2^v	42.318 (17)	Fe—O2—O1^vii	96.89 (2)
O2ⁱ—Fe—O2^v	137.681 (17)	O1—O2—O1^vii	71.37 (2)
O1ⁱⁱ—Fe—O2^v	67.134 (18)	O2^v—O2—O1^vii	62.49 (2)
O1ⁱⁱⁱ—Fe—O2^v	112.866 (18)	O1^v—O2—O1^vii	116.85 (2)
O3ⁱ—Fe—O2^v	119.766 (18)	O3^ix—O2—O1^vii	86.562 (18)
O3—Fe—O2^v	60.235 (18)	O1ⁱⁱⁱ—O2—O1^vii	79.398 (16)
O2ⁱⁱ—Fe—O2^v	84.210 (15)	O3ⁱ—O2—O1^vii	139.13 (2)
O2ⁱⁱⁱ—Fe—O2^v	95.790 (15)	O1ⁱⁱ—O2—O1^vii	109.24 (2)
O2^iv—Fe—O2^v	180.000 (12)	O3—O2—O1^vii	55.230 (12)
O1^v—S—O1	110.59 (4)	O1^xii—O2—O1^vii	142.146 (17)
O1^v—S—O2	110.05 (3)	Fe—O3—Fe^v	121.27 (3)
O1—S—O2	108.85 (3)	Fe—O3—O2^xiii	111.975 (14)
O1^v—S—O2^v	108.85 (3)	Fe^v—O3—O2^xiii	88.248 (13)
O1—S—O2^v	110.05 (3)	Fe—O3—O2ⁱⁱⁱ	88.248 (13)
O2—S—O2^v	108.42 (4)	Fe^v—O3—O2ⁱⁱⁱ	111.975 (14)
S—O1—Fe^vi	136.04 (3)	O2^xiii—O3—O2ⁱⁱⁱ	138.98 (3)
S—O1—O2	35.914 (16)	Fe—O3—O1ⁱⁱ	45.146 (13)
Fe^vi—O1—O2	100.22 (2)	Fe^v—O3—O1ⁱⁱ	103.47 (2)
S—O1—O1^v	34.70 (2)	O2^xiii—O3—O1ⁱⁱ	70.504 (17)
Fe^vi—O1—O1^v	139.79 (3)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	132.165 (15)
O2—O1—O1^v	60.412 (19)	Fe—O3—O1^vii	103.47 (2)
S—O1—O2^v	35.306 (17)	Fe^v—O3—O1^vii	45.146 (13)
Fe^vi—O1—O2^v	144.22 (3)	O2^xiii—O3—O1^vii	132.164 (15)
O2—O1—O2^v	60.12 (2)	O2ⁱⁱⁱ—O3—O1^vii	70.504 (16)
O1^v—O1—O2^v	59.675 (19)	O1ⁱⁱ—O3—O1^vii	122.41 (3)
S—O1—O2^vi	127.16 (3)	Fe—O3—O2^xiv	159.76 (2)
Fe^vi—O1—O2^vi	46.666 (13)	Fe^v—O3—O2^xiv	43.677 (11)
O2—O1—O2^vi	108.390 (19)	O2^xiii—O3—O2^xiv	83.726 (16)
O1^v—O1—O2^vi	102.85 (2)	O2ⁱⁱⁱ—O3—O2^xiv	87.459 (18)
O2^v—O1—O2^vi	161.84 (3)	O1ⁱⁱ—O3—O2^xiv	139.698 (16)
S—O1—O3^vii	171.03 (3)	O1^vii—O3—O2^xiv	56.532 (15)
Fe^vi—O1—O3^vii	48.319 (12)	Fe—O3—O2ⁱ	43.677 (11)
O2—O1—O3^vii	146.22 (2)	Fe^v—O3—O2ⁱ	159.76 (2)
O1^v—O1—O3^vii	150.223 (16)	O2^xiii—O3—O2ⁱ	87.459 (18)
O2^v—O1—O3^vii	135.81 (2)	O2ⁱⁱⁱ—O3—O2ⁱ	83.726 (16)
O2^vi—O1—O3^vii	61.808 (17)	O1ⁱⁱ—O3—O2ⁱ	56.532 (15)
S—O1—O2^viii	115.81 (3)	O1^vii—O3—O2ⁱ	139.698 (16)
Fe^vi—O1—O2^viii	41.839 (14)	O2^xiv—O3—O2ⁱ	154.67 (3)
O2—O1—O2^viii	87.400 (19)	Fe—O3—O2	41.846 (13)
O1^v—O1—O2^viii	147.744 (19)	Fe^v—O3—O2	80.97 (2)
O2^v—O1—O2^viii	104.10 (2)	O2^xiii—O3—O2	125.66 (2)
O2^vi—O1—O2^viii	88.50 (2)	O2ⁱⁱⁱ—O3—O2	93.523 (13)
O3^vii—O1—O2^viii	61.270 (19)	O1ⁱⁱ—O3—O2	60.958 (17)
S—O1—O3^ix	91.87 (2)	O1^vii—O3—O2	66.393 (18)
Fe^vi—O1—O3^ix	44.674 (13)	O2^xiv—O3—O2	118.768 (19)
O2—O1—O3^ix	56.968 (17)	O2ⁱ—O3—O2	85.523 (16)
O1^v—O1—O3^ix	101.78 (3)	Fe—O3—O2^v	80.97 (2)
O2^v—O1—O3^ix	114.19 (2)	Fe^v—O3—O2^v	41.846 (13)
O2^vi—O1—O3^ix	61.779 (18)	O2^xiii—O3—O2^v	93.522 (13)
O3^vii—O1—O3^ix	92.993 (18)	O2ⁱⁱⁱ—O3—O2^v	125.66 (2)
O2^viii—O1—O3^ix	57.065 (16)	O1ⁱⁱ—O3—O2^v	66.393 (19)
S—O1—O3^x	103.08 (3)	O1^vii—O3—O2^v	60.958 (17)
Fe^vi—O1—O3^x	97.544 (17)	O2^xiv—O3—O2^v	85.523 (15)
O2—O1—O3^x	118.53 (2)	O2ⁱ—O3—O2^v	118.768 (19)
O1^v—O1—O3^x	68.373 (10)	O2—O3—O2^v	46.25 (2)
O2^v—O1—O3^x	117.95 (2)	Fe—O3—O1^xiii	120.79 (2)
O2^vi—O1—O3^x	52.717 (15)	Fe^v—O3—O1^xiii	41.862 (10)
O3^vii—O1—O3^x	82.656 (16)	O2^xiii—O3—O1^xiii	47.548 (14)
O2^viii—O1—O3^x	137.388 (17)	O2ⁱⁱⁱ—O3—O1^xiii	147.279 (15)
O3^ix—O1—O3^x	107.210 (18)	O1ⁱⁱ—O3—O1^xiii	79.837 (16)
S—O1—O2^xi	126.76 (3)	O1^vii—O3—O1^xiii	87.008 (18)
Fe^vi—O1—O2^xi	96.725 (18)	O2^xiv—O3—O1^xiii	60.020 (15)
O2—O1—O2^xi	162.39 (3)	O2ⁱ—O3—O1^xiii	127.141 (14)
O1^v—O1—O2^xi	103.09 (2)	O2—O3—O1^xiii	98.96 (2)
O2^v—O1—O2^xi	107.42 (2)	O2^v—O3—O1^xiii	53.671 (13)
O2^vi—O1—O2^xi	80.062 (19)	Fe—O3—O1ⁱⁱⁱ	41.862 (10)
O3^vii—O1—O2^xi	51.372 (14)	Fe^v—O3—O1ⁱⁱⁱ	120.79 (2)
O2^viii—O1—O2^xi	108.62 (2)	O2^xiii—O3—O1ⁱⁱⁱ	147.279 (15)
O3^ix—O1—O2^xi	138.094 (19)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	47.548 (14)
O3^x—O1—O2^xi	53.857 (13)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	87.008 (18)
S—O1—O2^vii	113.23 (3)	O1^vii—O3—O1ⁱⁱⁱ	79.837 (16)
Fe^vi—O1—O2^vii	76.947 (19)	O2^xiv—O3—O1ⁱⁱⁱ	127.141 (14)
O2—O1—O2^vii	108.63 (2)	O2ⁱ—O3—O1ⁱⁱⁱ	60.020 (15)
O1^v—O1—O2^vii	140.60 (2)	O2—O3—O1ⁱⁱⁱ	53.672 (13)
O2^v—O1—O2^vii	81.724 (19)	O2^v—O3—O1ⁱⁱⁱ	98.96 (2)
O2^vi—O1—O2^vii	116.21 (2)	O1^xiii—O3—O1ⁱⁱⁱ	152.54 (3)
O3^vii—O1—O2^vii	58.376 (18)	Fe—O3—H	104.9 (10)
O2^viii—O1—O2^vii	44.321 (17)	Fe^v—O3—H	109.8 (10)
O3^ix—O1—O2^vii	101.046 (18)	O2^xiii—O3—H	121.2 (10)
O3^x—O1—O2^vii	132.677 (16)	O2ⁱⁱⁱ—O3—H	19.4 (10)
O2^xi—O1—O2^vii	79.800 (15)	O1ⁱⁱ—O3—H	144.7 (10)
S—O2—Fe	132.45 (3)	O1^vii—O3—H	76.7 (10)
S—O2—O1	35.238 (16)	O2^xiv—O3—H	75.3 (10)
Fe—O2—O1	162.31 (3)	O2ⁱ—O3—H	89.3 (10)
S—O2—O2^v	35.789 (19)	O2—O3—H	112.6 (10)
Fe—O2—O2^v	102.777 (17)	O2^v—O3—H	137.2 (10)
O1—O2—O2^v	60.307 (18)	O1^xiii—O3—H	133.9 (10)
S—O2—O1^v	34.645 (16)	O1ⁱⁱⁱ—O3—H	66.1 (10)
Fe—O2—O1^v	117.96 (2)	Fe—O3—H^v	109.8 (10)
O1—O2—O1^v	59.91 (3)	Fe^v—O3—H^v	104.9 (10)
O2^v—O2—O1^v	59.573 (18)	O2^xiii—O3—H^v	19.4 (10)
S—O2—O3^ix	109.50 (3)	O2ⁱⁱⁱ—O3—H^v	121.2 (10)
Fe—O2—O3^ix	117.96 (2)	O1ⁱⁱ—O3—H^v	76.7 (10)
O1—O2—O3^ix	75.48 (2)	O1^vii—O3—H^v	144.7 (10)
O2^v—O2—O3^ix	131.61 (3)	O2^xiv—O3—H^v	89.3 (10)
O1^v—O2—O3^ix	114.71 (3)	O2ⁱ—O3—H^v	75.3 (10)
S—O2—O1ⁱⁱⁱ	161.87 (3)	O2—O3—H^v	137.2 (10)
Fe—O2—O1ⁱⁱⁱ	48.290 (15)	O2^v—O3—H^v	112.6 (10)
O1—O2—O1ⁱⁱⁱ	137.25 (2)	O1^xiii—O3—H^v	66.1 (10)
O2^v—O2—O1ⁱⁱⁱ	129.661 (16)	O1ⁱⁱⁱ—O3—H^v	133.9 (10)
O1^v—O2—O1ⁱⁱⁱ	161.84 (3)	H—O3—H^v	105 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.850 (15)	1.950 (15)	2.7316 (6)	152.3 (14)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(FeSO4H2O_N2_153K) top

Crystal data top

FeH₂Mg₀O₅S	V = 363.74 (9) Å³
M_r = 169.93	Z = 4
Monoclinic, C2/c	F(000) = 336
a = 7.0482 (10) Å	D_x = 3.103 Mg m⁻³
b = 7.5706 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.7498 (10) Å	µ = 4.60 mm⁻¹
β = 118.404 (10)°	T = 153 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.023
T_min = 0.577, T_max = 0.748	θ_max = 40.0°, θ_min = 4.2°
10375 measured reflections	h = −12→12
1130 independent reflections	k = −13→13
1118 reflections with I > 2σ(I)	l = −14→14

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.013	w = 1/[σ²(F_o²) + (0.014P)² + 0.240P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.033	(Δ/σ)_max < 0.001
S = 1.18	Δρ_max = 0.55 e Å⁻³
1130 reflections	Δρ_min = −0.50 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0219 (12)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe	0.000000	0.500000	0.000000	0.00477 (4)
S	0.000000	0.15482 (2)	0.250000	0.00421 (4)
O1	0.16858 (7)	0.04450 (7)	0.40013 (7)	0.00847 (7)
O2	0.09931 (7)	0.26982 (6)	0.15882 (7)	0.00747 (7)
O3	0.000000	0.64402 (9)	0.250000	0.00722 (9)
H	0.107 (2)	0.716 (2)	0.294 (2)	0.025 (4)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe	0.00440 (5)	0.00465 (5)	0.00517 (5)	0.00000 (3)	0.00221 (4)	0.00056 (3)
S	0.00323 (7)	0.00388 (7)	0.00537 (7)	0.000	0.00192 (5)	0.000
O1	0.00528 (15)	0.00941 (17)	0.00988 (16)	0.00255 (13)	0.00292 (13)	0.00441 (13)
O2	0.00714 (15)	0.00668 (15)	0.01017 (16)	0.00053 (12)	0.00539 (13)	0.00284 (12)
O3	0.0070 (2)	0.0074 (2)	0.0076 (2)	0.000	0.00373 (18)	0.000

Geometric parameters (Å, º) top

Fe—O2	2.0547 (5)	O1—O1^v	2.4086 (10)
Fe—O2ⁱ	2.0547 (5)	O1—O2^v	2.4214 (7)
Fe—O1ⁱⁱ	2.1093 (6)	O1—O2^vi	2.8143 (7)
Fe—O1ⁱⁱⁱ	2.1093 (6)	O1—O3^vii	2.9698 (7)
Fe—O3ⁱ	2.2232 (4)	O1—O2^viii	3.0694 (8)
Fe—O3	2.2232 (4)	O1—O3^ix	3.1565 (6)
Fe—O2ⁱⁱ	3.4692 (6)	O1—O3^x	3.2623 (9)
Fe—O2ⁱⁱⁱ	3.4692 (6)	O1—O2^xi	3.2941 (7)
Fe—O2^iv	3.5041 (6)	O1—O2^vii	3.3189 (8)
Fe—O2^v	3.5041 (6)	O2—O2^v	2.4165 (9)
S—O1^v	1.4655 (5)	O2—O3^ix	2.7356 (6)
S—O1	1.4656 (5)	O2—O3ⁱ	2.9738 (6)
S—O2^v	1.4892 (5)	O2—O3	3.0798 (8)
S—O2	1.4892 (5)	O3—H	0.856 (16)
O1—O2	2.4035 (7)	O3—H^v	0.856 (16)

O2—Fe—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	71.99 (2)
O2—Fe—O1ⁱⁱ	94.97 (2)	S—O2—O3ⁱ	135.09 (3)
O2ⁱ—Fe—O1ⁱⁱ	85.03 (2)	Fe—O2—O3ⁱ	48.342 (16)
O2—Fe—O1ⁱⁱⁱ	85.03 (2)	O1—O2—O3ⁱ	147.39 (3)
O2ⁱ—Fe—O1ⁱⁱⁱ	94.97 (2)	O2^v—O2—O3ⁱ	135.63 (3)
O1ⁱⁱ—Fe—O1ⁱⁱⁱ	180.0	O1^v—O2—O3ⁱ	100.73 (2)
O2—Fe—O3ⁱ	87.99 (2)	O3^ix—O2—O3ⁱ	92.432 (18)
O2ⁱ—Fe—O3ⁱ	92.01 (2)	O1ⁱⁱⁱ—O2—O3ⁱ	61.666 (17)
O1ⁱⁱ—Fe—O3ⁱ	93.496 (16)	S—O2—O1ⁱⁱ	92.04 (2)
O1ⁱⁱⁱ—Fe—O3ⁱ	86.504 (16)	Fe—O2—O1ⁱⁱ	43.205 (13)
O2—Fe—O3	92.01 (2)	O1—O2—O1ⁱⁱ	127.22 (3)
O2ⁱ—Fe—O3	87.99 (2)	O2^v—O2—O1ⁱⁱ	73.37 (2)
O1ⁱⁱ—Fe—O3	86.504 (16)	O1^v—O2—O1ⁱⁱ	76.06 (2)
O1ⁱⁱⁱ—Fe—O3	93.496 (16)	O3^ix—O2—O1ⁱⁱ	155.09 (2)
O3ⁱ—Fe—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	91.51 (2)
O2—Fe—O2ⁱⁱ	83.052 (13)	O3ⁱ—O2—O1ⁱⁱ	62.952 (16)
O2ⁱ—Fe—O2ⁱⁱ	96.948 (14)	S—O2—O3	102.68 (2)
O1ⁱⁱ—Fe—O2ⁱⁱ	42.975 (16)	Fe—O2—O3	46.171 (13)
O1ⁱⁱⁱ—Fe—O2ⁱⁱ	137.025 (16)	O1—O2—O3	117.29 (2)
O3ⁱ—Fe—O2ⁱⁱ	52.011 (12)	O2^v—O2—O3	66.902 (10)
O3—Fe—O2ⁱⁱ	127.989 (12)	O1^v—O2—O3	116.70 (2)
O2—Fe—O2ⁱⁱⁱ	96.948 (13)	O3^ix—O2—O3	125.48 (2)
O2ⁱ—Fe—O2ⁱⁱⁱ	83.052 (14)	O1ⁱⁱⁱ—O2—O3	64.576 (17)
O1ⁱⁱ—Fe—O2ⁱⁱⁱ	137.025 (16)	O3ⁱ—O2—O3	94.513 (16)
O1ⁱⁱⁱ—Fe—O2ⁱⁱⁱ	42.975 (16)	O1ⁱⁱ—O2—O3	57.757 (13)
O3ⁱ—Fe—O2ⁱⁱⁱ	127.989 (13)	S—O2—O1^xii	96.06 (2)
O3—Fe—O2ⁱⁱⁱ	52.011 (12)	Fe—O2—O1^xii	110.79 (2)
O2ⁱⁱ—Fe—O2ⁱⁱⁱ	180.0	O1—O2—O1^xii	85.802 (17)
O2—Fe—O2^iv	137.762 (17)	O2^v—O2—O1^xii	130.597 (15)
O2ⁱ—Fe—O2^iv	42.238 (17)	O1^v—O2—O1^xii	72.80 (2)
O1ⁱⁱ—Fe—O2^iv	112.732 (19)	O3^ix—O2—O1^xii	58.133 (17)
O1ⁱⁱⁱ—Fe—O2^iv	67.268 (19)	O1ⁱⁱⁱ—O2—O1^xii	99.735 (19)
O3ⁱ—Fe—O2^iv	60.231 (18)	O3ⁱ—O2—O1^xii	62.482 (19)
O3—Fe—O2^iv	119.769 (18)	O1ⁱⁱ—O2—O1^xii	108.67 (2)
O2ⁱⁱ—Fe—O2^iv	95.746 (16)	O3—O2—O1^xii	156.891 (19)
O2ⁱⁱⁱ—Fe—O2^iv	84.254 (16)	S—O2—O1^vii	82.62 (2)
O2—Fe—O2^v	42.238 (17)	Fe—O2—O1^vii	96.79 (2)
O2ⁱ—Fe—O2^v	137.762 (17)	O1—O2—O1^vii	71.40 (2)
O1ⁱⁱ—Fe—O2^v	67.268 (19)	O2^v—O2—O1^vii	62.39 (2)
O1ⁱⁱⁱ—Fe—O2^v	112.732 (19)	O1^v—O2—O1^vii	116.80 (2)
O3ⁱ—Fe—O2^v	119.769 (18)	O3^ix—O2—O1^vii	86.496 (19)
O3—Fe—O2^v	60.231 (18)	O1ⁱⁱⁱ—O2—O1^vii	79.305 (16)
O2ⁱⁱ—Fe—O2^v	84.254 (16)	O3ⁱ—O2—O1^vii	139.04 (2)
O2ⁱⁱⁱ—Fe—O2^v	95.746 (15)	O1ⁱⁱ—O2—O1^vii	109.18 (2)
O2^iv—Fe—O2^v	180.0	O3—O2—O1^vii	55.154 (13)
O1^v—S—O1	110.52 (4)	O1^xii—O2—O1^vii	142.145 (18)
O1^v—S—O2^v	108.86 (3)	Fe—O3—Fe^v	121.26 (3)
O1—S—O2^v	110.06 (3)	Fe—O3—O2^xiii	111.938 (14)
O1^v—S—O2	110.06 (3)	Fe^v—O3—O2^xiii	88.160 (13)
O1—S—O2	108.86 (3)	Fe—O3—O2ⁱⁱⁱ	88.160 (13)
O2^v—S—O2	108.45 (4)	Fe^v—O3—O2ⁱⁱⁱ	111.938 (14)
S—O1—Fe^vi	136.09 (3)	O2^xiii—O3—O2ⁱⁱⁱ	139.25 (3)
S—O1—O2	35.897 (16)	Fe—O3—O1ⁱⁱ	45.147 (13)
Fe^vi—O1—O2	100.28 (2)	Fe^v—O3—O1ⁱⁱ	103.53 (2)
S—O1—O1^v	34.74 (2)	O2^xiii—O3—O1ⁱⁱ	70.395 (17)
Fe^vi—O1—O1^v	139.99 (3)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	132.079 (16)
O2—O1—O1^v	60.42 (2)	Fe—O3—O1^vii	103.53 (2)
S—O1—O2^v	35.291 (17)	Fe^v—O3—O1^vii	45.147 (13)
Fe^vi—O1—O2^v	144.08 (3)	O2^xiii—O3—O1^vii	132.079 (15)
O2—O1—O2^v	60.11 (2)	O2ⁱⁱⁱ—O3—O1^vii	70.395 (17)
O1^v—O1—O2^v	59.685 (19)	O1ⁱⁱ—O3—O1^vii	122.55 (3)
S—O1—O2^vi	127.34 (3)	Fe—O3—O2^xiv	159.79 (2)
Fe^vi—O1—O2^vi	46.665 (14)	Fe^v—O3—O2^xiv	43.671 (11)
O2—O1—O2^vi	108.46 (2)	O2^xiii—O3—O2^xiv	83.668 (17)
O1^v—O1—O2^vi	103.05 (2)	O2ⁱⁱⁱ—O3—O2^xiv	87.568 (18)
O2^v—O1—O2^vi	162.03 (3)	O1ⁱⁱ—O3—O2^xiv	139.677 (17)
S—O1—O3^vii	170.84 (3)	O1^vii—O3—O2^xiv	56.524 (15)
Fe^vi—O1—O3^vii	48.349 (12)	Fe—O3—O2ⁱ	43.671 (11)
O2—O1—O3^vii	146.29 (2)	Fe^v—O3—O2ⁱ	159.79 (2)
O1^v—O1—O3^vii	150.245 (17)	O2^xiii—O3—O2ⁱ	87.568 (18)
O2^v—O1—O3^vii	135.64 (2)	O2ⁱⁱⁱ—O3—O2ⁱ	83.668 (17)
O2^vi—O1—O3^vii	61.811 (17)	O1ⁱⁱ—O3—O2ⁱ	56.524 (15)
S—O1—O2^viii	115.72 (3)	O1^vii—O3—O2ⁱ	139.677 (17)
Fe^vi—O1—O2^viii	41.828 (14)	O2^xiv—O3—O2ⁱ	154.66 (3)
O2—O1—O2^viii	87.41 (2)	Fe—O3—O2	41.817 (14)
O1^v—O1—O2^viii	147.76 (2)	Fe^v—O3—O2	80.97 (2)
O2^v—O1—O2^viii	103.94 (2)	O2^xiii—O3—O2	125.48 (2)
O2^vi—O1—O2^viii	88.49 (2)	O2ⁱⁱⁱ—O3—O2	93.447 (14)
O3^vii—O1—O2^viii	61.297 (19)	O1ⁱⁱ—O3—O2	60.947 (18)
S—O1—O3^ix	91.95 (2)	O1^vii—O3—O2	66.516 (19)
Fe^vi—O1—O3^ix	44.668 (13)	O2^xiv—O3—O2	118.83 (2)
O2—O1—O3^ix	57.032 (18)	O2ⁱ—O3—O2	85.487 (16)
O1^v—O1—O3^ix	101.94 (3)	Fe—O3—O2^v	80.97 (2)
O2^v—O1—O3^ix	114.18 (2)	Fe^v—O3—O2^v	41.817 (14)
O2^vi—O1—O3^ix	61.789 (18)	O2^xiii—O3—O2^v	93.447 (14)
O3^vii—O1—O3^ix	93.018 (18)	O2ⁱⁱⁱ—O3—O2^v	125.48 (2)
O2^viii—O1—O3^ix	57.043 (16)	O1ⁱⁱ—O3—O2^v	66.516 (19)
S—O1—O3^x	103.08 (3)	O1^vii—O3—O2^v	60.947 (18)
Fe^vi—O1—O3^x	97.719 (18)	O2^xiv—O3—O2^v	85.487 (16)
O2—O1—O3^x	118.51 (2)	O2ⁱ—O3—O2^v	118.83 (2)
O1^v—O1—O3^x	68.337 (10)	O2—O3—O2^v	46.20 (2)
O2^v—O1—O3^x	117.93 (2)	Fe—O3—O1^xiii	120.73 (2)
O2^vi—O1—O3^x	52.887 (15)	Fe^v—O3—O1^xiii	41.835 (11)
O3^vii—O1—O3^x	82.752 (17)	O2^xiii—O3—O1^xiii	47.487 (15)
O2^viii—O1—O3^x	137.548 (18)	O2ⁱⁱⁱ—O3—O1^xiii	147.347 (15)
O3^ix—O1—O3^x	107.350 (18)	O1ⁱⁱ—O3—O1^xiii	79.818 (16)
S—O1—O2^xi	126.58 (3)	O1^vii—O3—O1^xiii	86.983 (18)
Fe^vi—O1—O2^xi	96.903 (19)	O2^xiv—O3—O1^xiii	60.004 (15)
O2—O1—O2^xi	162.21 (3)	O2ⁱ—O3—O1^xiii	127.203 (15)
O1^v—O1—O2^xi	102.96 (2)	O2—O3—O1^xiii	98.85 (2)
O2^v—O1—O2^xi	107.20 (2)	O2^v—O3—O1^xiii	53.635 (14)
O2^vi—O1—O2^xi	80.27 (2)	Fe—O3—O1ⁱⁱⁱ	41.835 (11)
O3^vii—O1—O2^xi	51.472 (15)	Fe^v—O3—O1ⁱⁱⁱ	120.73 (2)
O2^viii—O1—O2^xi	108.68 (2)	O2^xiii—O3—O1ⁱⁱⁱ	147.347 (15)
O3^ix—O1—O2^xi	138.30 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	47.487 (14)
O3^x—O1—O2^xi	53.944 (14)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	86.983 (18)
S—O1—O2^vii	113.11 (3)	O1^vii—O3—O1ⁱⁱⁱ	79.818 (16)
Fe^vi—O1—O2^vii	76.848 (19)	O2^xiv—O3—O1ⁱⁱⁱ	127.203 (15)
O2—O1—O2^vii	108.60 (2)	O2ⁱ—O3—O1ⁱⁱⁱ	60.004 (15)
O1^v—O1—O2^vii	140.48 (2)	O2—O3—O1ⁱⁱⁱ	53.635 (14)
O2^v—O1—O2^vii	81.609 (19)	O2^v—O3—O1ⁱⁱⁱ	98.85 (2)
O2^vi—O1—O2^vii	116.12 (2)	O1^xiii—O3—O1ⁱⁱⁱ	152.38 (3)
O3^vii—O1—O2^vii	58.331 (18)	Fe—O3—H	107.0 (11)
O2^viii—O1—O2^vii	44.237 (17)	Fe^v—O3—H	109.3 (10)
O3^ix—O1—O2^vii	100.944 (19)	O2^xiii—O3—H	119.0 (11)
O3^x—O1—O2^vii	132.719 (17)	O2ⁱⁱⁱ—O3—H	22.0 (11)
O2^xi—O1—O2^vii	79.767 (16)	O1ⁱⁱ—O3—H	145.9 (10)
S—O2—Fe	132.61 (3)	O1^vii—O3—H	77.5 (10)
S—O2—O1	35.240 (16)	O2^xiv—O3—H	73.8 (10)
Fe—O2—O1	162.41 (3)	O2ⁱ—O3—H	90.0 (10)
S—O2—O2^v	35.776 (19)	O2—O3—H	115.0 (11)
Fe—O2—O2^v	102.902 (18)	O2^v—O3—H	138.3 (11)
O1—O2—O2^v	60.312 (19)	O1^xiii—O3—H	132.1 (10)
S—O2—O1^v	34.648 (17)	O1ⁱⁱⁱ—O3—H	68.5 (11)
Fe—O2—O1^v	118.14 (3)	Fe—O3—H^v	109.3 (10)
O1—O2—O1^v	59.89 (3)	Fe^v—O3—H^v	107.0 (11)
O2^v—O2—O1^v	59.579 (18)	O2^xiii—O3—H^v	22.0 (11)
S—O2—O3^ix	109.54 (3)	O2ⁱⁱⁱ—O3—H^v	119.0 (11)
Fe—O2—O3^ix	117.75 (2)	O1ⁱⁱ—O3—H^v	77.5 (10)
O1—O2—O3^ix	75.48 (2)	O1^vii—O3—H^v	145.9 (10)
O2^v—O2—O3^ix	131.53 (3)	O2^xiv—O3—H^v	90.0 (10)
O1^v—O2—O3^ix	114.84 (3)	O2ⁱ—O3—H^v	73.8 (10)
S—O2—O1ⁱⁱⁱ	161.75 (3)	O2—O3—H^v	138.3 (11)
Fe—O2—O1ⁱⁱⁱ	48.302 (16)	O2^v—O3—H^v	115.0 (11)
O1—O2—O1ⁱⁱⁱ	137.06 (2)	O1^xiii—O3—H^v	68.5 (11)
O2^v—O2—O1ⁱⁱⁱ	129.655 (16)	O1ⁱⁱⁱ—O3—H^v	132.1 (11)
O1^v—O2—O1ⁱⁱⁱ	162.03 (3)	H—O3—H^v	101 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.856 (16)	1.968 (15)	2.7356 (6)	148.6 (15)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(FeSO4H2O_N2_193K) top

Crystal data top

FeH₂Mg₀O₅S	V = 364.23 (9) Å³
M_r = 169.93	Z = 4
Monoclinic, C2/c	F(000) = 336
a = 7.058 (1) Å	D_x = 3.099 Mg m⁻³
b = 7.5663 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.7576 (10) Å	µ = 4.60 mm⁻¹
β = 118.454 (10)°	T = 193 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.026
T_min = 0.572, T_max = 0.748	θ_max = 40.0°, θ_min = 4.2°
10377 measured reflections	h = −12→12
1131 independent reflections	k = −13→13
1112 reflections with I > 2σ(I)	l = −14→14

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.013	w = 1/[σ²(F_o²) + (0.015P)² + 0.2P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.034	(Δ/σ)_max < 0.001
S = 1.17	Δρ_max = 0.49 e Å⁻³
1131 reflections	Δρ_min = −0.51 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0331 (14)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe	0.000000	0.500000	0.000000	0.00582 (4)
S	0.000000	0.15447 (2)	0.250000	0.00507 (4)
O1	0.16874 (7)	0.04405 (7)	0.39968 (7)	0.01016 (8)
O2	0.09854 (7)	0.26941 (6)	0.15838 (7)	0.00889 (7)
O3	0.000000	0.64418 (9)	0.250000	0.00850 (9)
H	0.108 (2)	0.716 (2)	0.294 (2)	0.028 (4)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe	0.00531 (5)	0.00572 (5)	0.00630 (5)	−0.00003 (3)	0.00266 (4)	0.00064 (3)
S	0.00382 (7)	0.00462 (7)	0.00651 (7)	0.000	0.00225 (5)	0.000
O1	0.00629 (15)	0.01111 (17)	0.01199 (17)	0.00299 (13)	0.00347 (13)	0.00538 (14)
O2	0.00832 (15)	0.00798 (15)	0.01216 (17)	0.00074 (12)	0.00633 (13)	0.00344 (13)
O3	0.0084 (2)	0.0088 (2)	0.0087 (2)	0.000	0.00439 (18)	0.000

Geometric parameters (Å, º) top

Fe—O2	2.0550 (5)	O1—O1^v	2.4074 (10)
Fe—O2ⁱ	2.0551 (5)	O1—O2^v	2.4206 (7)
Fe—O1ⁱⁱ	2.1093 (6)	O1—O2^vi	2.8150 (7)
Fe—O1ⁱⁱⁱ	2.1093 (6)	O1—O3^vii	2.9708 (7)
Fe—O3ⁱ	2.2252 (4)	O1—O2^viii	3.0694 (8)
Fe—O3	2.2252 (4)	O1—O3^ix	3.1584 (6)
Fe—O2ⁱⁱ	3.4715 (6)	O1—O3^x	3.2562 (9)
Fe—O2ⁱⁱⁱ	3.4715 (6)	O1—O2^xi	3.2932 (7)
Fe—O2^iv	3.5082 (6)	O1—O2^vii	3.3284 (8)
Fe—O2^v	3.5082 (6)	O2—O2^v	2.4166 (9)
S—O1	1.4652 (5)	O2—O3^ix	2.7409 (6)
S—O1^v	1.4652 (5)	O2—O3ⁱ	2.9745 (6)
S—O2^v	1.4887 (5)	O2—O3	3.0824 (8)
S—O2	1.4887 (5)	O3—H	0.865 (16)
O1—O2	2.4027 (7)	O3—H^v	0.865 (16)

O2—Fe—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	71.74 (2)
O2—Fe—O1ⁱⁱ	94.95 (2)	S—O2—O3ⁱ	135.36 (3)
O2ⁱ—Fe—O1ⁱⁱ	85.05 (2)	Fe—O2—O3ⁱ	48.382 (16)
O2—Fe—O1ⁱⁱⁱ	85.05 (2)	O1—O2—O3ⁱ	147.41 (3)
O2ⁱ—Fe—O1ⁱⁱⁱ	94.95 (2)	O2^v—O2—O3ⁱ	135.93 (3)
O1ⁱⁱ—Fe—O1ⁱⁱⁱ	180.0	O1^v—O2—O3ⁱ	100.99 (2)
O2—Fe—O3ⁱ	87.95 (2)	O3^ix—O2—O3ⁱ	92.317 (18)
O2ⁱ—Fe—O3ⁱ	92.05 (2)	O1ⁱⁱⁱ—O2—O3ⁱ	61.674 (17)
O1ⁱⁱ—Fe—O3ⁱ	93.511 (16)	S—O2—O1ⁱⁱ	92.28 (2)
O1ⁱⁱⁱ—Fe—O3ⁱ	86.489 (16)	Fe—O2—O1ⁱⁱ	43.208 (13)
O2—Fe—O3	92.05 (2)	O1—O2—O1ⁱⁱ	127.48 (3)
O2ⁱ—Fe—O3	87.95 (2)	O2^v—O2—O1ⁱⁱ	73.62 (2)
O1ⁱⁱ—Fe—O3	86.489 (16)	O1^v—O2—O1ⁱⁱ	76.26 (2)
O1ⁱⁱⁱ—Fe—O3	93.511 (17)	O3^ix—O2—O1ⁱⁱ	154.97 (2)
O3ⁱ—Fe—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	91.50 (2)
O2—Fe—O2ⁱⁱ	83.023 (13)	O3ⁱ—O2—O1ⁱⁱ	62.987 (16)
O2ⁱ—Fe—O2ⁱⁱ	96.977 (14)	S—O2—O3	102.66 (2)
O1ⁱⁱ—Fe—O2ⁱⁱ	42.903 (16)	Fe—O2—O3	46.173 (13)
O1ⁱⁱⁱ—Fe—O2ⁱⁱ	137.097 (16)	O1—O2—O3	117.30 (2)
O3ⁱ—Fe—O2ⁱⁱ	52.100 (12)	O2^v—O2—O3	66.921 (10)
O3—Fe—O2ⁱⁱ	127.900 (12)	O1^v—O2—O3	116.71 (2)
O2—Fe—O2ⁱⁱⁱ	96.977 (13)	O3^ix—O2—O3	125.25 (2)
O2ⁱ—Fe—O2ⁱⁱⁱ	83.023 (13)	O1ⁱⁱⁱ—O2—O3	64.579 (16)
O1ⁱⁱ—Fe—O2ⁱⁱⁱ	137.097 (16)	O3ⁱ—O2—O3	94.555 (16)
O1ⁱⁱⁱ—Fe—O2ⁱⁱⁱ	42.903 (16)	O1ⁱⁱ—O2—O3	57.752 (13)
O3ⁱ—Fe—O2ⁱⁱⁱ	127.900 (12)	S—O2—O1^xii	96.34 (3)
O3—Fe—O2ⁱⁱⁱ	52.099 (12)	Fe—O2—O1^xii	110.70 (2)
O2ⁱⁱ—Fe—O2ⁱⁱⁱ	180.0	O1—O2—O1^xii	85.909 (17)
O2—Fe—O2^iv	137.854 (17)	O2^v—O2—O1^xii	130.871 (15)
O2ⁱ—Fe—O2^iv	42.145 (17)	O1^v—O2—O1^xii	73.11 (2)
O1ⁱⁱ—Fe—O2^iv	112.562 (19)	O3^ix—O2—O1^xii	58.129 (17)
O1ⁱⁱⁱ—Fe—O2^iv	67.438 (19)	O1ⁱⁱⁱ—O2—O1^xii	99.52 (2)
O3ⁱ—Fe—O2^iv	60.205 (18)	O3ⁱ—O2—O1^xii	62.354 (19)
O3—Fe—O2^iv	119.795 (18)	O1ⁱⁱ—O2—O1^xii	108.75 (2)
O2ⁱⁱ—Fe—O2^iv	95.671 (16)	O3—O2—O1^xii	156.786 (19)
O2ⁱⁱⁱ—Fe—O2^iv	84.329 (15)	S—O2—O1^vii	82.50 (2)
O2—Fe—O2^v	42.146 (17)	Fe—O2—O1^vii	96.67 (2)
O2ⁱ—Fe—O2^v	137.855 (17)	O1—O2—O1^vii	71.40 (2)
O1ⁱⁱ—Fe—O2^v	67.438 (19)	O2^v—O2—O1^vii	62.22 (2)
O1ⁱⁱⁱ—Fe—O2^v	112.562 (19)	O1^v—O2—O1^vii	116.66 (2)
O3ⁱ—Fe—O2^v	119.795 (18)	O3^ix—O2—O1^vii	86.425 (19)
O3—Fe—O2^v	60.205 (18)	O1ⁱⁱⁱ—O2—O1^vii	79.195 (16)
O2ⁱⁱ—Fe—O2^v	84.329 (16)	O3ⁱ—O2—O1^vii	138.94 (2)
O2ⁱⁱⁱ—Fe—O2^v	95.671 (15)	O1ⁱⁱ—O2—O1^vii	109.11 (2)
O2^iv—Fe—O2^v	180.0	O3—O2—O1^vii	55.052 (13)
O1—S—O1^v	110.47 (4)	O1^xii—O2—O1^vii	142.132 (18)
O1—S—O2^v	110.06 (3)	Fe—O3—Fe^v	121.28 (3)
O1^v—S—O2^v	108.86 (3)	Fe—O3—O2ⁱⁱⁱ	88.063 (13)
O1—S—O2	108.86 (3)	Fe^v—O3—O2ⁱⁱⁱ	111.885 (14)
O1^v—S—O2	110.06 (3)	Fe—O3—O2^xiii	111.885 (14)
O2^v—S—O2	108.52 (4)	Fe^v—O3—O2^xiii	88.063 (13)
S—O1—Fe^vi	136.22 (3)	O2ⁱⁱⁱ—O3—O2^xiii	139.55 (3)
S—O1—O2	35.897 (16)	Fe—O3—O1ⁱⁱ	45.128 (13)
Fe^vi—O1—O2	100.40 (2)	Fe^v—O3—O1ⁱⁱ	103.62 (2)
S—O1—O1^v	34.77 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	131.968 (16)
Fe^vi—O1—O1^v	140.29 (3)	O2^xiii—O3—O1ⁱⁱ	70.288 (17)
O2—O1—O1^v	60.43 (2)	Fe—O3—O1^vii	103.62 (2)
S—O1—O2^v	35.289 (17)	Fe^v—O3—O1^vii	45.128 (13)
Fe^vi—O1—O2^v	143.95 (3)	O2ⁱⁱⁱ—O3—O1^vii	70.289 (17)
O2—O1—O2^v	60.13 (2)	O2^xiii—O3—O1^vii	131.967 (16)
O1^v—O1—O2^v	59.691 (19)	O1ⁱⁱ—O3—O1^vii	122.71 (3)
S—O1—O2^vi	127.60 (3)	Fe—O3—O2^xiv	159.87 (2)
Fe^vi—O1—O2^vi	46.662 (14)	Fe^v—O3—O2^xiv	43.664 (11)
O2—O1—O2^vi	108.58 (2)	O2ⁱⁱⁱ—O3—O2^xiv	87.684 (18)
O1^v—O1—O2^vi	103.31 (2)	O2^xiii—O3—O2^xiv	83.595 (17)
O2^v—O1—O2^vi	162.30 (3)	O1ⁱⁱ—O3—O2^xiv	139.678 (17)
S—O1—O3^vii	170.59 (3)	O1^vii—O3—O2^xiv	56.519 (16)
Fe^vi—O1—O3^vii	48.383 (12)	Fe—O3—O2ⁱ	43.664 (11)
O2—O1—O3^vii	146.43 (2)	Fe^v—O3—O2ⁱ	159.87 (2)
O1^v—O1—O3^vii	150.246 (17)	O2ⁱⁱⁱ—O3—O2ⁱ	83.595 (17)
O2^v—O1—O3^vii	135.38 (2)	O2^xiii—O3—O2ⁱ	87.684 (18)
O2^vi—O1—O3^vii	61.808 (17)	O1ⁱⁱ—O3—O2ⁱ	56.519 (16)
S—O1—O2^viii	115.65 (3)	O1^vii—O3—O2ⁱ	139.678 (17)
Fe^vi—O1—O2^viii	41.839 (14)	O2^xiv—O3—O2ⁱ	154.60 (3)
O2—O1—O2^viii	87.46 (2)	Fe—O3—O2	41.780 (14)
O1^v—O1—O2^viii	147.79 (2)	Fe^v—O3—O2	81.00 (2)
O2^v—O1—O2^viii	103.74 (2)	O2ⁱⁱⁱ—O3—O2	93.374 (13)
O2^vi—O1—O2^viii	88.50 (2)	O2^xiii—O3—O2	125.25 (2)
O3^vii—O1—O2^viii	61.344 (19)	O1ⁱⁱ—O3—O2	60.904 (18)
S—O1—O3^ix	92.09 (2)	O1^vii—O3—O2	66.686 (19)
Fe^vi—O1—O3^ix	44.684 (12)	O2^xiv—O3—O2	118.94 (2)
O2—O1—O3^ix	57.135 (18)	O2ⁱ—O3—O2	85.444 (16)
O1^v—O1—O3^ix	102.17 (3)	Fe—O3—O2^v	81.00 (2)
O2^v—O1—O3^ix	114.23 (2)	Fe^v—O3—O2^v	41.780 (14)
O2^vi—O1—O3^ix	61.815 (19)	O2ⁱⁱⁱ—O3—O2^v	125.25 (2)
O3^vii—O1—O3^ix	93.067 (18)	O2^xiii—O3—O2^v	93.373 (14)
O2^viii—O1—O3^ix	57.040 (16)	O1ⁱⁱ—O3—O2^v	66.685 (19)
S—O1—O3^x	103.07 (3)	O1^vii—O3—O2^v	60.904 (18)
Fe^vi—O1—O3^x	97.906 (18)	O2^xiv—O3—O2^v	85.445 (16)
O2—O1—O3^x	118.49 (2)	O2ⁱ—O3—O2^v	118.94 (2)
O1^v—O1—O3^x	68.305 (10)	O2—O3—O2^v	46.16 (2)
O2^v—O1—O3^x	117.90 (2)	Fe—O3—O1^xiii	120.68 (2)
O2^vi—O1—O3^x	53.072 (16)	Fe^v—O3—O1^xiii	41.805 (11)
O3^vii—O1—O3^x	82.848 (17)	O2ⁱⁱⁱ—O3—O1^xiii	147.402 (15)
O2^viii—O1—O3^x	137.737 (18)	O2^xiii—O3—O1^xiii	47.419 (14)
O3^ix—O1—O3^x	107.508 (19)	O1ⁱⁱ—O3—O1^xiii	79.835 (16)
S—O1—O2^xi	126.31 (3)	O1^vii—O3—O1^xiii	86.932 (18)
Fe^vi—O1—O2^xi	97.095 (19)	O2^xiv—O3—O1^xiii	59.973 (15)
O2—O1—O2^xi	161.95 (3)	O2ⁱ—O3—O1^xiii	127.291 (15)
O1^v—O1—O2^xi	102.76 (2)	O2—O3—O1^xiii	98.74 (2)
O2^v—O1—O2^xi	106.89 (2)	O2^v—O3—O1^xiii	53.606 (14)
O2^vi—O1—O2^xi	80.476 (19)	Fe—O3—O1ⁱⁱⁱ	41.805 (11)
O3^vii—O1—O2^xi	51.583 (15)	Fe^v—O3—O1ⁱⁱⁱ	120.68 (2)
O2^viii—O1—O2^xi	108.75 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	47.420 (14)
O3^ix—O1—O2^xi	138.54 (2)	O2^xiii—O3—O1ⁱⁱⁱ	147.403 (15)
O3^x—O1—O2^xi	54.020 (14)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	86.932 (18)
S—O1—O2^vii	112.98 (3)	O1^vii—O3—O1ⁱⁱⁱ	79.835 (17)
Fe^vi—O1—O2^vii	76.743 (19)	O2^xiv—O3—O1ⁱⁱⁱ	127.291 (15)
O2—O1—O2^vii	108.60 (2)	O2ⁱ—O3—O1ⁱⁱⁱ	59.973 (15)
O1^v—O1—O2^vii	140.31 (2)	O2—O3—O1ⁱⁱⁱ	53.605 (14)
O2^v—O1—O2^vii	81.45 (2)	O2^v—O3—O1ⁱⁱⁱ	98.74 (2)
O2^vi—O1—O2^vii	116.02 (2)	O1^xiii—O3—O1ⁱⁱⁱ	152.24 (3)
O3^vii—O1—O2^vii	58.262 (18)	Fe—O3—H	106.8 (10)
O2^viii—O1—O2^vii	44.154 (18)	Fe^v—O3—H	109.4 (10)
O3^ix—O1—O2^vii	100.865 (19)	O2ⁱⁱⁱ—O3—H	21.9 (10)
O3^x—O1—O2^vii	132.726 (17)	O2^xiii—O3—H	119.4 (11)
O2^xi—O1—O2^vii	79.711 (15)	O1ⁱⁱ—O3—H	145.7 (10)
S—O2—Fe	132.79 (3)	O1^vii—O3—H	77.3 (10)
S—O2—O1	35.246 (16)	O2^xiv—O3—H	74.1 (10)
Fe—O2—O1	162.50 (3)	O2ⁱ—O3—H	89.8 (10)
S—O2—O2^v	35.742 (19)	O2—O3—H	114.8 (11)
Fe—O2—O2^v	103.061 (17)	O2^v—O3—H	138.1 (10)
O1—O2—O2^v	60.299 (19)	O1^xiii—O3—H	132.3 (10)
S—O2—O1^v	34.652 (17)	O1ⁱⁱⁱ—O3—H	68.3 (10)
Fe—O2—O1^v	118.36 (3)	Fe—O3—H^v	109.4 (10)
O1—O2—O1^v	59.88 (3)	Fe^v—O3—H^v	106.8 (10)
O2^v—O2—O1^v	59.565 (18)	O2ⁱⁱⁱ—O3—H^v	119.4 (11)
S—O2—O3^ix	109.55 (3)	O2^xiii—O3—H^v	21.9 (11)
Fe—O2—O3^ix	117.52 (2)	O1ⁱⁱ—O3—H^v	77.3 (10)
O1—O2—O3^ix	75.45 (2)	O1^vii—O3—H^v	145.7 (10)
O2^v—O2—O3^ix	131.39 (3)	O2^xiv—O3—H^v	89.8 (10)
O1^v—O2—O3^ix	114.99 (3)	O2ⁱ—O3—H^v	74.1 (10)
S—O2—O1ⁱⁱⁱ	161.54 (3)	O2—O3—H^v	138.1 (10)
Fe—O2—O1ⁱⁱⁱ	48.292 (16)	O2^v—O3—H^v	114.8 (11)
O1—O2—O1ⁱⁱⁱ	136.81 (2)	O1^xiii—O3—H^v	68.3 (10)
O2^v—O2—O1ⁱⁱⁱ	129.598 (17)	O1ⁱⁱⁱ—O3—H^v	132.3 (10)
O1^v—O2—O1ⁱⁱⁱ	162.30 (3)	H—O3—H^v	102 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.865 (16)	1.965 (15)	2.7409 (6)	148.7 (15)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(FeSO4H2O_N2_233K) top

Crystal data top

FeH₂Mg₀O₅S	V = 364.85 (9) Å³
M_r = 169.93	Z = 4
Monoclinic, C2/c	F(000) = 336
a = 7.0696 (10) Å	D_x = 3.094 Mg m⁻³
b = 7.562 (1) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.7669 (10) Å	µ = 4.59 mm⁻¹
β = 118.515 (10)°	T = 233 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.031
T_min = 0.561, T_max = 0.748	θ_max = 40.0°, θ_min = 4.2°
10393 measured reflections	h = −12→12
1133 independent reflections	k = −13→13
1117 reflections with I > 2σ(I)	l = −14→14

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.013	w = 1/[σ²(F_o²) + (0.017P)² + 0.170P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.035	(Δ/σ)_max < 0.001
S = 1.15	Δρ_max = 0.55 e Å⁻³
1133 reflections	Δρ_min = −0.54 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.079 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe	0.000000	0.500000	0.000000	0.00700 (4)
S	0.000000	0.15406 (2)	0.250000	0.00601 (4)
O1	0.16893 (7)	0.04355 (7)	0.39918 (7)	0.01200 (8)
O2	0.09766 (7)	0.26893 (6)	0.15794 (7)	0.01060 (8)
O3	0.000000	0.64450 (9)	0.250000	0.00989 (10)
H	0.105 (3)	0.718 (2)	0.295 (2)	0.034 (4)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe	0.00634 (5)	0.00685 (6)	0.00754 (6)	−0.00004 (3)	0.00310 (4)	0.00074 (3)
S	0.00456 (7)	0.00540 (7)	0.00768 (7)	0.000	0.00260 (5)	0.000
O1	0.00723 (15)	0.01321 (18)	0.01418 (18)	0.00356 (14)	0.00400 (13)	0.00646 (15)
O2	0.01009 (16)	0.00930 (16)	0.01444 (18)	0.00102 (12)	0.00749 (14)	0.00417 (13)
O3	0.0099 (2)	0.0102 (2)	0.0099 (2)	0.000	0.00501 (18)	0.000

Geometric parameters (Å, º) top

Fe—O2	2.0557 (5)	O1—O1^v	2.4063 (10)
Fe—O2ⁱ	2.0558 (5)	O1—O2^v	2.4197 (7)
Fe—O1ⁱⁱ	2.1095 (6)	O1—O2^vi	2.8163 (7)
Fe—O1ⁱⁱⁱ	2.1095 (6)	O1—O3^vii	2.9725 (7)
Fe—O3	2.2281 (4)	O1—O2^viii	3.0693 (8)
Fe—O3ⁱ	2.2281 (4)	O1—O3^ix	3.1611 (6)
Fe—O2ⁱⁱ	3.4741 (6)	O1—O3^x	3.2486 (9)
Fe—O2ⁱⁱⁱ	3.4741 (6)	O1—O2^xi	3.2930 (7)
Fe—O2^iv	3.5127 (6)	O1—O2^vii	3.3386 (9)
Fe—O2^v	3.5127 (6)	O2—O2^v	2.4159 (9)
S—O1^v	1.4649 (5)	O2—O3^ix	2.7469 (6)
S—O1	1.4649 (5)	O2—O3ⁱ	2.9758 (6)
S—O2^v	1.4879 (5)	O2—O3	3.0863 (8)
S—O2	1.4879 (5)	O3—H	0.857 (17)
O1—O2	2.4017 (7)	O3—H^v	0.857 (17)

O2—Fe—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	71.45 (2)
O2—Fe—O1ⁱⁱ	94.93 (2)	S—O2—O3ⁱ	135.65 (3)
O2ⁱ—Fe—O1ⁱⁱ	85.07 (2)	Fe—O2—O3ⁱ	48.437 (16)
O2—Fe—O1ⁱⁱⁱ	85.07 (2)	O1—O2—O3ⁱ	147.39 (3)
O2ⁱ—Fe—O1ⁱⁱⁱ	94.93 (2)	O2^v—O2—O3ⁱ	136.27 (3)
O1ⁱⁱ—Fe—O1ⁱⁱⁱ	180.0	O1^v—O2—O3ⁱ	101.26 (2)
O2—Fe—O3	92.09 (2)	O3^ix—O2—O3ⁱ	92.154 (18)
O2ⁱ—Fe—O3	87.91 (2)	O1ⁱⁱⁱ—O2—O3ⁱ	61.682 (18)
O1ⁱⁱ—Fe—O3	86.472 (16)	S—O2—O1ⁱⁱ	92.56 (2)
O1ⁱⁱⁱ—Fe—O3	93.528 (17)	Fe—O2—O1ⁱⁱ	43.215 (13)
O2—Fe—O3ⁱ	87.91 (2)	O1—O2—O1ⁱⁱ	127.77 (3)
O2ⁱ—Fe—O3ⁱ	92.09 (2)	O2^v—O2—O1ⁱⁱ	73.91 (2)
O1ⁱⁱ—Fe—O3ⁱ	93.528 (16)	O1^v—O2—O1ⁱⁱ	76.47 (2)
O1ⁱⁱⁱ—Fe—O3ⁱ	86.472 (16)	O3^ix—O2—O1ⁱⁱ	154.80 (2)
O3—Fe—O3ⁱ	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	91.48 (2)
O2—Fe—O2ⁱⁱ	82.987 (13)	O3ⁱ—O2—O1ⁱⁱ	63.034 (17)
O2ⁱ—Fe—O2ⁱⁱ	97.013 (14)	S—O2—O3	102.68 (2)
O1ⁱⁱ—Fe—O2ⁱⁱ	42.816 (16)	Fe—O2—O3	46.174 (12)
O1ⁱⁱⁱ—Fe—O2ⁱⁱ	137.184 (16)	O1—O2—O3	117.33 (2)
O3—Fe—O2ⁱⁱ	127.799 (12)	O2^v—O2—O3	66.958 (10)
O3ⁱ—Fe—O2ⁱⁱ	52.201 (12)	O1^v—O2—O3	116.73 (2)
O2—Fe—O2ⁱⁱⁱ	97.013 (13)	O3^ix—O2—O3	124.98 (2)
O2ⁱ—Fe—O2ⁱⁱⁱ	82.987 (13)	O1ⁱⁱⁱ—O2—O3	64.573 (17)
O1ⁱⁱ—Fe—O2ⁱⁱⁱ	137.183 (16)	O3ⁱ—O2—O3	94.611 (16)
O1ⁱⁱⁱ—Fe—O2ⁱⁱⁱ	42.817 (16)	O1ⁱⁱ—O2—O3	57.748 (13)
O3—Fe—O2ⁱⁱⁱ	52.200 (12)	S—O2—O1^xii	96.64 (3)
O3ⁱ—Fe—O2ⁱⁱⁱ	127.800 (12)	Fe—O2—O1^xii	110.57 (2)
O2ⁱⁱ—Fe—O2ⁱⁱⁱ	180.0	O1—O2—O1^xii	86.025 (18)
O2—Fe—O2^iv	137.974 (17)	O2^v—O2—O1^xii	131.183 (15)
O2ⁱ—Fe—O2^iv	42.025 (17)	O1^v—O2—O1^xii	73.47 (2)
O1ⁱⁱ—Fe—O2^iv	112.38 (2)	O3^ix—O2—O1^xii	58.125 (17)
O1ⁱⁱⁱ—Fe—O2^iv	67.62 (2)	O1ⁱⁱⁱ—O2—O1^xii	99.27 (2)
O3—Fe—O2^iv	119.797 (19)	O3ⁱ—O2—O1^xii	62.183 (19)
O3ⁱ—Fe—O2^iv	60.204 (19)	O1ⁱⁱ—O2—O1^xii	108.84 (2)
O2ⁱⁱ—Fe—O2^iv	95.601 (15)	O3—O2—O1^xii	156.644 (19)
O2ⁱⁱⁱ—Fe—O2^iv	84.400 (15)	S—O2—O1^vii	82.38 (2)
O2—Fe—O2^v	42.026 (17)	Fe—O2—O1^vii	96.53 (2)
O2ⁱ—Fe—O2^v	137.975 (17)	O1—O2—O1^vii	71.41 (2)
O1ⁱⁱ—Fe—O2^v	67.62 (2)	O2^v—O2—O1^vii	62.04 (2)
O1ⁱⁱⁱ—Fe—O2^v	112.38 (2)	O1^v—O2—O1^vii	116.53 (2)
O3—Fe—O2^v	60.203 (19)	O3^ix—O2—O1^vii	86.344 (19)
O3ⁱ—Fe—O2^v	119.796 (19)	O1ⁱⁱⁱ—O2—O1^vii	79.078 (17)
O2ⁱⁱ—Fe—O2^v	84.399 (15)	O3ⁱ—O2—O1^vii	138.84 (2)
O2ⁱⁱⁱ—Fe—O2^v	95.600 (16)	O1ⁱⁱ—O2—O1^vii	109.04 (2)
O2^iv—Fe—O2^v	180.0	O3—O2—O1^vii	54.946 (13)
O1^v—S—O1	110.43 (5)	O1^xii—O2—O1^vii	142.114 (18)
O1^v—S—O2^v	108.85 (3)	Fe—O3—Fe^v	121.26 (3)
O1—S—O2^v	110.06 (3)	Fe—O3—O2ⁱⁱⁱ	87.939 (13)
O1^v—S—O2	110.06 (3)	Fe^v—O3—O2ⁱⁱⁱ	111.836 (15)
O1—S—O2	108.85 (3)	Fe—O3—O2^xiii	111.836 (15)
O2^v—S—O2	108.56 (4)	Fe^v—O3—O2^xiii	87.938 (13)
S—O1—Fe^vi	136.37 (3)	O2ⁱⁱⁱ—O3—O2^xiii	139.94 (3)
S—O1—O2	35.896 (17)	Fe—O3—O1ⁱⁱ	45.098 (13)
Fe^vi—O1—O2	100.53 (2)	Fe^v—O3—O1ⁱⁱ	103.69 (2)
S—O1—O1^v	34.78 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	131.824 (16)
Fe^vi—O1—O1^v	140.61 (4)	O2^xiii—O3—O1ⁱⁱ	70.178 (18)
O2—O1—O1^v	60.43 (2)	Fe—O3—O1^vii	103.69 (2)
S—O1—O2^v	35.280 (18)	Fe^v—O3—O1^vii	45.098 (13)
Fe^vi—O1—O2^v	143.81 (3)	O2ⁱⁱⁱ—O3—O1^vii	70.178 (18)
O2—O1—O2^v	60.14 (3)	O2^xiii—O3—O1^vii	131.823 (16)
O1^v—O1—O2^v	59.69 (2)	O1ⁱⁱ—O3—O1^vii	122.84 (3)
S—O1—O2^vi	127.86 (3)	Fe—O3—O2^xiv	159.93 (2)
Fe^vi—O1—O2^vi	46.657 (14)	Fe^v—O3—O2^xiv	43.658 (12)
O2—O1—O2^vi	108.71 (2)	O2ⁱⁱⁱ—O3—O2^xiv	87.846 (18)
O1^v—O1—O2^vi	103.60 (2)	O2^xiii—O3—O2^xiv	83.503 (17)
O2^v—O1—O2^vi	162.58 (3)	O1ⁱⁱ—O3—O2^xiv	139.656 (17)
S—O1—O3^vii	170.33 (3)	O1^vii—O3—O2^xiv	56.517 (16)
Fe^vi—O1—O3^vii	48.430 (12)	Fe—O3—O2ⁱ	43.658 (12)
O2—O1—O3^vii	146.59 (2)	Fe^v—O3—O2ⁱ	159.93 (2)
O1^v—O1—O3^vii	150.225 (17)	O2ⁱⁱⁱ—O3—O2ⁱ	83.504 (17)
O2^v—O1—O3^vii	135.12 (3)	O2^xiii—O3—O2ⁱ	87.847 (18)
O2^vi—O1—O3^vii	61.802 (17)	O1ⁱⁱ—O3—O2ⁱ	56.517 (16)
S—O1—O2^viii	115.58 (3)	O1^vii—O3—O2ⁱ	139.656 (17)
Fe^vi—O1—O2^viii	41.860 (15)	O2^xiv—O3—O2ⁱ	154.58 (3)
O2—O1—O2^viii	87.52 (2)	Fe—O3—O2^v	81.01 (2)
O1^v—O1—O2^viii	147.83 (2)	Fe^v—O3—O2^v	41.733 (14)
O2^v—O1—O2^viii	103.52 (2)	O2ⁱⁱⁱ—O3—O2^v	124.98 (2)
O2^vi—O1—O2^viii	88.52 (2)	O2^xiii—O3—O2^v	93.277 (14)
O3^vii—O1—O2^viii	61.413 (19)	O1ⁱⁱ—O3—O2^v	66.85 (2)
S—O1—O3^ix	92.24 (2)	O1^vii—O3—O2^v	60.839 (19)
Fe^vi—O1—O3^ix	44.709 (13)	O2^xiv—O3—O2^v	85.390 (16)
O2—O1—O3^ix	57.244 (18)	O2ⁱ—O3—O2^v	119.03 (2)
O1^v—O1—O3^ix	102.43 (3)	Fe—O3—O2	41.732 (14)
O2^v—O1—O3^ix	114.26 (2)	Fe^v—O3—O2	81.01 (2)
O2^vi—O1—O3^ix	61.855 (19)	O2ⁱⁱⁱ—O3—O2	93.277 (14)
O3^vii—O1—O3^ix	93.139 (18)	O2^xiii—O3—O2	124.98 (2)
O2^viii—O1—O3^ix	57.039 (16)	O1ⁱⁱ—O3—O2	60.839 (18)
S—O1—O3^x	103.04 (3)	O1^vii—O3—O2	66.85 (2)
Fe^vi—O1—O3^x	98.118 (19)	O2^xiv—O3—O2	119.03 (2)
O2—O1—O3^x	118.45 (2)	O2ⁱ—O3—O2	85.390 (16)
O1^v—O1—O3^x	68.262 (10)	O2^v—O3—O2	46.08 (2)
O2^v—O1—O3^x	117.86 (2)	Fe—O3—O1^xiii	120.60 (2)
O2^vi—O1—O3^x	53.284 (16)	Fe^v—O3—O1^xiii	41.763 (11)
O3^vii—O1—O3^x	82.940 (17)	O2ⁱⁱⁱ—O3—O1^xiii	147.479 (15)
O2^viii—O1—O3^x	137.960 (19)	O2^xiii—O3—O1^xiii	47.331 (14)
O3^ix—O1—O3^x	107.701 (19)	O1ⁱⁱ—O3—O1^xiii	79.845 (16)
S—O1—O2^xi	125.99 (3)	O1^vii—O3—O1^xiii	86.861 (19)
Fe^vi—O1—O2^xi	97.317 (19)	O2^xiv—O3—O1^xiii	59.927 (16)
O2—O1—O2^xi	161.65 (3)	O2ⁱ—O3—O1^xiii	127.398 (15)
O1^v—O1—O2^xi	102.53 (2)	O2^v—O3—O1^xiii	53.573 (14)
O2^v—O1—O2^xi	106.54 (2)	O2—O3—O1^xiii	98.59 (2)
O2^vi—O1—O2^xi	80.73 (2)	Fe—O3—O1ⁱⁱⁱ	41.763 (11)
O3^vii—O1—O2^xi	51.698 (15)	Fe^v—O3—O1ⁱⁱⁱ	120.60 (2)
O2^viii—O1—O2^xi	108.84 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	47.332 (14)
O3^ix—O1—O2^xi	138.83 (2)	O2^xiii—O3—O1ⁱⁱⁱ	147.480 (15)
O3^x—O1—O2^xi	54.114 (14)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	86.861 (19)
S—O1—O2^vii	112.83 (3)	O1^vii—O3—O1ⁱⁱⁱ	79.845 (16)
Fe^vi—O1—O2^vii	76.630 (19)	O2^xiv—O3—O1ⁱⁱⁱ	127.398 (15)
O2—O1—O2^vii	108.59 (2)	O2ⁱ—O3—O1ⁱⁱⁱ	59.927 (15)
O1^v—O1—O2^vii	140.12 (2)	O2^v—O3—O1ⁱⁱⁱ	98.59 (2)
O2^v—O1—O2^vii	81.28 (2)	O2—O3—O1ⁱⁱⁱ	53.572 (14)
O2^vi—O1—O2^vii	115.91 (2)	O1^xiii—O3—O1ⁱⁱⁱ	152.05 (3)
O3^vii—O1—O2^vii	58.207 (19)	Fe—O3—H	108.1 (11)
O2^viii—O1—O2^vii	44.048 (18)	Fe^v—O3—H	108.8 (11)
O3^ix—O1—O2^vii	100.766 (19)	O2ⁱⁱⁱ—O3—H	23.4 (11)
O3^x—O1—O2^vii	132.745 (17)	O2^xiii—O3—H	118.4 (11)
O2^xi—O1—O2^vii	79.650 (15)	O1ⁱⁱ—O3—H	146.5 (11)
S—O2—Fe	133.02 (3)	O1^vii—O3—H	77.5 (11)
S—O2—O1	35.258 (17)	O2^xiv—O3—H	73.1 (11)
Fe—O2—O1	162.62 (3)	O2ⁱ—O3—H	90.4 (11)
S—O2—O2^v	35.72 (2)	O2^v—O3—H	138.2 (11)
Fe—O2—O2^v	103.248 (18)	O2—O3—H	116.1 (11)
O1—O2—O2^v	60.30 (2)	O1^xiii—O3—H	131.1 (11)
S—O2—O1^v	34.656 (18)	O1ⁱⁱⁱ—O3—H	69.7 (11)
Fe—O2—O1^v	118.62 (3)	Fe—O3—H^v	108.8 (11)
O1—O2—O1^v	59.88 (3)	Fe^v—O3—H^v	108.1 (11)
O2^v—O2—O1^v	59.556 (19)	O2ⁱⁱⁱ—O3—H^v	118.4 (11)
S—O2—O3^ix	109.59 (3)	O2^xiii—O3—H^v	23.4 (11)
Fe—O2—O3^ix	117.23 (2)	O1ⁱⁱ—O3—H^v	77.5 (11)
O1—O2—O3^ix	75.42 (2)	O1^vii—O3—H^v	146.5 (11)
O2^v—O2—O3^ix	131.25 (3)	O2^xiv—O3—H^v	90.4 (11)
O1^v—O2—O3^ix	115.19 (3)	O2ⁱ—O3—H^v	73.1 (11)
S—O2—O1ⁱⁱⁱ	161.33 (3)	O2^v—O3—H^v	116.1 (11)
Fe—O2—O1ⁱⁱⁱ	48.268 (16)	O2—O3—H^v	138.2 (11)
O1—O2—O1ⁱⁱⁱ	136.53 (2)	O1^xiii—O3—H^v	69.7 (11)
O2^v—O2—O1ⁱⁱⁱ	129.544 (17)	O1ⁱⁱⁱ—O3—H^v	131.1 (11)
O1^v—O2—O1ⁱⁱⁱ	162.58 (3)	H—O3—H^v	100 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.857 (17)	1.989 (16)	2.7469 (6)	146.8 (16)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(FeSO4H2O_N2_273K) top

Crystal data top

FeH₂Mg₀O₅S	V = 365.31 (9) Å³
M_r = 169.93	Z = 4
Monoclinic, C2/c	F(000) = 336
a = 7.0802 (10) Å	D_x = 3.090 Mg m⁻³
b = 7.5565 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.7755 (10) Å	µ = 4.58 mm⁻¹
β = 118.579 (10)°	T = 273 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.032
T_min = 0.550, T_max = 0.748	θ_max = 40.0°, θ_min = 4.2°
10420 measured reflections	h = −12→12
1137 independent reflections	k = −13→13
1117 reflections with I > 2σ(I)	l = −14→14

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.014	w = 1/[σ²(F_o²) + (0.018P)² + 0.170P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.036	(Δ/σ)_max < 0.001
S = 1.10	Δρ_max = 0.51 e Å⁻³
1137 reflections	Δρ_min = −0.83 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.231 (4)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe	0.000000	0.500000	0.000000	0.00810 (4)
S	0.000000	0.15360 (2)	0.250000	0.00688 (5)
O1	0.16920 (7)	0.04295 (7)	0.39860 (8)	0.01391 (8)
O2	0.09661 (7)	0.26840 (6)	0.15737 (7)	0.01223 (8)
O3	0.000000	0.64461 (9)	0.250000	0.01132 (10)
H	0.106 (3)	0.718 (2)	0.296 (2)	0.037 (4)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe	0.00734 (6)	0.00813 (6)	0.00863 (6)	−0.00008 (3)	0.00365 (4)	0.00083 (3)
S	0.00523 (7)	0.00633 (7)	0.00873 (7)	0.000	0.00305 (5)	0.000
O1	0.00844 (16)	0.01536 (19)	0.01643 (19)	0.00421 (14)	0.00475 (14)	0.00751 (16)
O2	0.01166 (16)	0.01093 (17)	0.01664 (19)	0.00136 (13)	0.00882 (15)	0.00494 (14)
O3	0.0115 (2)	0.0120 (2)	0.0110 (2)	0.000	0.00587 (19)	0.000

Geometric parameters (Å, º) top

Fe—O2	2.0560 (5)	O1—O1^v	2.4048 (11)
Fe—O2ⁱ	2.0560 (5)	O1—O2^v	2.4187 (7)
Fe—O1ⁱⁱ	2.1085 (6)	O1—O2^vi	2.8166 (7)
Fe—O1ⁱⁱⁱ	2.1085 (6)	O1—O3^vii	2.9728 (7)
Fe—O3	2.2299 (4)	O1—O2^viii	3.0680 (8)
Fe—O3ⁱ	2.2300 (4)	O1—O3^ix	3.1623 (6)
Fe—O2ⁱⁱ	3.4768 (6)	O1—O3^x	3.2414 (9)
Fe—O2ⁱⁱⁱ	3.4769 (6)	O1—O2^xi	3.2920 (8)
Fe—O2^iv	3.5173 (6)	O1—O2^vii	3.3503 (9)
Fe—O2^v	3.5173 (6)	O2—O2^v	2.4149 (9)
S—O1^v	1.4646 (5)	O2—O3^ix	2.7537 (6)
S—O1	1.4646 (5)	O2—O3ⁱ	2.9766 (6)
S—O2	1.4868 (5)	O2—O3	3.0886 (9)
S—O2^v	1.4868 (5)	O3—H	0.863 (17)
O1—O2	2.4005 (7)	O3—H^v	0.863 (17)

O2—Fe—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	71.16 (2)
O2—Fe—O1ⁱⁱ	94.89 (2)	S—O2—O3ⁱ	136.02 (3)
O2ⁱ—Fe—O1ⁱⁱ	85.11 (2)	Fe—O2—O3ⁱ	48.473 (16)
O2—Fe—O1ⁱⁱⁱ	85.11 (2)	O1—O2—O3ⁱ	147.41 (3)
O2ⁱ—Fe—O1ⁱⁱⁱ	94.89 (2)	O2^v—O2—O3ⁱ	136.67 (3)
O1ⁱⁱ—Fe—O1ⁱⁱⁱ	180.0	O1^v—O2—O3ⁱ	101.60 (2)
O2—Fe—O3	92.12 (2)	O3^ix—O2—O3ⁱ	92.003 (19)
O2ⁱ—Fe—O3	87.88 (2)	O1ⁱⁱⁱ—O2—O3ⁱ	61.674 (18)
O1ⁱⁱ—Fe—O3	86.456 (17)	S—O2—O1ⁱⁱ	92.91 (2)
O1ⁱⁱⁱ—Fe—O3	93.544 (17)	Fe—O2—O1ⁱⁱ	43.216 (14)
O2—Fe—O3ⁱ	87.88 (2)	O1—O2—O1ⁱⁱ	128.14 (3)
O2ⁱ—Fe—O3ⁱ	92.12 (2)	O2^v—O2—O1ⁱⁱ	74.26 (2)
O1ⁱⁱ—Fe—O3ⁱ	93.544 (16)	O1^v—O2—O1ⁱⁱ	76.75 (3)
O1ⁱⁱⁱ—Fe—O3ⁱ	86.456 (16)	O3^ix—O2—O1ⁱⁱ	154.63 (2)
O3—Fe—O3ⁱ	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	91.45 (2)
O2—Fe—O2ⁱⁱ	82.933 (13)	O3ⁱ—O2—O1ⁱⁱ	63.066 (17)
O2ⁱ—Fe—O2ⁱⁱ	97.067 (13)	S—O2—O3	102.68 (3)
O1ⁱⁱ—Fe—O2ⁱⁱ	42.719 (17)	Fe—O2—O3	46.179 (13)
O1ⁱⁱⁱ—Fe—O2ⁱⁱ	137.281 (17)	O1—O2—O3	117.36 (2)
O3—Fe—O2ⁱⁱ	127.679 (13)	O2^v—O2—O3	66.987 (10)
O3ⁱ—Fe—O2ⁱⁱ	52.320 (12)	O1^v—O2—O3	116.76 (2)
O2—Fe—O2ⁱⁱⁱ	97.067 (14)	O3^ix—O2—O3	124.71 (2)
O2ⁱ—Fe—O2ⁱⁱⁱ	82.933 (13)	O1ⁱⁱⁱ—O2—O3	64.564 (18)
O1ⁱⁱ—Fe—O2ⁱⁱⁱ	137.281 (17)	O3ⁱ—O2—O3	94.652 (16)
O1ⁱⁱⁱ—Fe—O2ⁱⁱⁱ	42.719 (17)	O1ⁱⁱ—O2—O3	57.743 (14)
O3—Fe—O2ⁱⁱⁱ	52.321 (12)	S—O2—O1^xii	96.99 (3)
O3ⁱ—Fe—O2ⁱⁱⁱ	127.679 (13)	Fe—O2—O1^xii	110.45 (2)
O2ⁱⁱ—Fe—O2ⁱⁱⁱ	180.000 (17)	O1—O2—O1^xii	86.141 (18)
O2—Fe—O2^iv	138.110 (17)	O2^v—O2—O1^xii	131.544 (16)
O2ⁱ—Fe—O2^iv	41.890 (17)	O1^v—O2—O1^xii	73.87 (2)
O1ⁱⁱ—Fe—O2^iv	112.15 (2)	O3^ix—O2—O1^xii	58.092 (17)
O1ⁱⁱⁱ—Fe—O2^iv	67.85 (2)	O1ⁱⁱⁱ—O2—O1^xii	99.00 (2)
O3—Fe—O2^iv	119.838 (19)	O3ⁱ—O2—O1^xii	62.03 (2)
O3ⁱ—Fe—O2^iv	60.163 (19)	O1ⁱⁱ—O2—O1^xii	108.94 (2)
O2ⁱⁱ—Fe—O2^iv	95.508 (16)	O3—O2—O1^xii	156.50 (2)
O2ⁱⁱⁱ—Fe—O2^iv	84.492 (16)	S—O2—O1^vii	82.22 (2)
O2—Fe—O2^v	41.890 (17)	Fe—O2—O1^vii	96.37 (2)
O2ⁱ—Fe—O2^v	138.110 (17)	O1—O2—O1^vii	71.42 (3)
O1ⁱⁱ—Fe—O2^v	67.85 (2)	O2^v—O2—O1^vii	61.81 (2)
O1ⁱⁱⁱ—Fe—O2^v	112.15 (2)	O1^v—O2—O1^vii	116.36 (3)
O3—Fe—O2^v	60.162 (19)	O3^ix—O2—O1^vii	86.268 (19)
O3ⁱ—Fe—O2^v	119.837 (19)	O1ⁱⁱⁱ—O2—O1^vii	78.936 (17)
O2ⁱⁱ—Fe—O2^v	84.492 (16)	O3ⁱ—O2—O1^vii	138.69 (2)
O2ⁱⁱⁱ—Fe—O2^v	95.508 (16)	O1ⁱⁱ—O2—O1^vii	108.95 (2)
O2^iv—Fe—O2^v	180.0	O3—O2—O1^vii	54.810 (13)
O1^v—S—O1	110.37 (5)	O1^xii—O2—O1^vii	142.086 (19)
O1^v—S—O2	110.07 (3)	Fe—O3—Fe^v	121.32 (3)
O1—S—O2	108.85 (3)	Fe—O3—O2^xiii	111.776 (15)
O1^v—S—O2^v	108.85 (3)	Fe^v—O3—O2^xiii	87.820 (13)
O1—S—O2^v	110.07 (3)	Fe—O3—O2ⁱⁱⁱ	87.820 (13)
O2—S—O2^v	108.61 (4)	Fe^v—O3—O2ⁱⁱⁱ	111.775 (15)
S—O1—Fe^vi	136.55 (3)	O2^xiii—O3—O2ⁱⁱⁱ	140.28 (3)
S—O1—O2	35.884 (17)	Fe—O3—O1ⁱⁱ	45.066 (13)
Fe^vi—O1—O2	100.70 (2)	Fe^v—O3—O1ⁱⁱ	103.83 (2)
S—O1—O1^v	34.81 (2)	O2^xiii—O3—O1ⁱⁱ	70.063 (18)
Fe^vi—O1—O1^v	141.00 (4)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	131.676 (16)
O2—O1—O1^v	60.44 (2)	Fe—O3—O1^vii	103.83 (2)
S—O1—O2^v	35.266 (19)	Fe^v—O3—O1^vii	45.066 (14)
Fe^vi—O1—O2^v	143.63 (3)	O2^xiii—O3—O1^vii	131.676 (16)
O2—O1—O2^v	60.15 (3)	O2ⁱⁱⁱ—O3—O1^vii	70.062 (18)
O1^v—O1—O2^v	59.69 (2)	O1ⁱⁱ—O3—O1^vii	123.05 (3)
S—O1—O2^vi	128.20 (3)	Fe—O3—O2^xiv	160.05 (3)
Fe^vi—O1—O2^vi	46.660 (15)	Fe^v—O3—O2^xiv	43.649 (12)
O2—O1—O2^vi	108.89 (2)	O2^xiii—O3—O2^xiv	83.392 (18)
O1^v—O1—O2^vi	103.95 (2)	O2ⁱⁱⁱ—O3—O2^xiv	87.996 (18)
O2^v—O1—O2^vi	162.93 (3)	O1ⁱⁱ—O3—O2^xiv	139.668 (17)
S—O1—O3^vii	169.99 (3)	O1^vii—O3—O2^xiv	56.514 (17)
Fe^vi—O1—O3^vii	48.477 (12)	Fe—O3—O2ⁱ	43.649 (12)
O2—O1—O3^vii	146.78 (3)	Fe^v—O3—O2ⁱ	160.05 (3)
O1^v—O1—O3^vii	150.219 (18)	O2^xiii—O3—O2ⁱ	87.996 (19)
O2^v—O1—O3^vii	134.77 (3)	O2ⁱⁱⁱ—O3—O2ⁱ	83.392 (17)
O2^vi—O1—O3^vii	61.812 (18)	O1ⁱⁱ—O3—O2ⁱ	56.514 (17)
S—O1—O2^viii	115.47 (3)	O1^vii—O3—O2ⁱ	139.668 (18)
Fe^vi—O1—O2^viii	41.889 (15)	O2^xiv—O3—O2ⁱ	154.48 (3)
O2—O1—O2^viii	87.59 (2)	Fe—O3—O2	41.699 (14)
O1^v—O1—O2^viii	147.88 (2)	Fe^v—O3—O2	81.06 (2)
O2^v—O1—O2^viii	103.25 (3)	O2^xiii—O3—O2	124.71 (2)
O2^vi—O1—O2^viii	88.55 (2)	O2ⁱⁱⁱ—O3—O2	93.209 (14)
O3^vii—O1—O2^viii	61.48 (2)	O1ⁱⁱ—O3—O2	60.781 (19)
S—O1—O3^ix	92.43 (3)	O1^vii—O3—O2	67.08 (2)
Fe^vi—O1—O3^ix	44.735 (13)	O2^xiv—O3—O2	119.18 (2)
O2—O1—O3^ix	57.402 (19)	O2ⁱ—O3—O2	85.349 (16)
O1^v—O1—O3^ix	102.74 (3)	Fe—O3—O2^v	81.06 (2)
O2^v—O1—O3^ix	114.31 (3)	Fe^v—O3—O2^v	41.699 (14)
O2^vi—O1—O3^ix	61.888 (19)	O2^xiii—O3—O2^v	93.209 (14)
O3^vii—O1—O3^ix	93.213 (19)	O2ⁱⁱⁱ—O3—O2^v	124.71 (2)
O2^viii—O1—O3^ix	57.055 (16)	O1ⁱⁱ—O3—O2^v	67.08 (2)
S—O1—O3^x	103.04 (3)	O1^vii—O3—O2^v	60.781 (19)
Fe^vi—O1—O3^x	98.36 (2)	O2^xiv—O3—O2^v	85.349 (17)
O2—O1—O3^x	118.43 (3)	O2ⁱ—O3—O2^v	119.18 (2)
O1^v—O1—O3^x	68.225 (10)	O2—O3—O2^v	46.03 (2)
O2^v—O1—O3^x	117.83 (2)	Fe—O3—O1^xiii	120.55 (2)
O2^vi—O1—O3^x	53.517 (16)	Fe^v—O3—O1^xiii	41.721 (11)
O3^vii—O1—O3^x	83.063 (18)	O2^xiii—O3—O1^xiii	47.256 (15)
O2^viii—O1—O3^x	138.216 (19)	O2ⁱⁱⁱ—O3—O1^xiii	147.539 (16)
O3^ix—O1—O3^x	107.90 (2)	O1ⁱⁱ—O3—O1^xiii	79.888 (17)
S—O1—O2^xi	125.61 (3)	O1^vii—O3—O1^xiii	86.788 (19)
Fe^vi—O1—O2^xi	97.57 (2)	O2^xiv—O3—O1^xiii	59.879 (16)
O2—O1—O2^xi	161.28 (3)	O2ⁱ—O3—O1^xiii	127.526 (16)
O1^v—O1—O2^xi	102.25 (2)	O2—O3—O1^xiii	98.45 (2)
O2^v—O1—O2^xi	106.13 (2)	O2^v—O3—O1^xiii	53.548 (15)
O2^vi—O1—O2^xi	81.00 (2)	Fe—O3—O1ⁱⁱⁱ	41.721 (11)
O3^vii—O1—O2^xi	51.846 (16)	Fe^v—O3—O1ⁱⁱⁱ	120.55 (2)
O2^viii—O1—O2^xi	108.94 (2)	O2^xiii—O3—O1ⁱⁱⁱ	147.539 (16)
O3^ix—O1—O2^xi	139.15 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	47.256 (15)
O3^x—O1—O2^xi	54.201 (14)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	86.788 (19)
S—O1—O2^vii	112.64 (3)	O1^vii—O3—O1ⁱⁱⁱ	79.888 (17)
Fe^vi—O1—O2^vii	76.50 (2)	O2^xiv—O3—O1ⁱⁱⁱ	127.526 (16)
O2—O1—O2^vii	108.58 (3)	O2ⁱ—O3—O1ⁱⁱⁱ	59.879 (16)
O1^v—O1—O2^vii	139.88 (3)	O2—O3—O1ⁱⁱⁱ	53.548 (15)
O2^v—O1—O2^vii	81.06 (2)	O2^v—O3—O1ⁱⁱⁱ	98.45 (2)
O2^vi—O1—O2^vii	115.78 (2)	O1^xiii—O3—O1ⁱⁱⁱ	151.88 (3)
O3^vii—O1—O2^vii	58.113 (19)	Fe—O3—H	108.3 (11)
O2^viii—O1—O2^vii	43.930 (18)	Fe^v—O3—H	108.5 (11)
O3^ix—O1—O2^vii	100.67 (2)	O2^xiii—O3—H	118.7 (12)
O3^x—O1—O2^vii	132.750 (18)	O2ⁱⁱⁱ—O3—H	23.6 (11)
O2^xi—O1—O2^vii	79.586 (16)	O1ⁱⁱ—O3—H	146.7 (11)
S—O2—Fe	133.30 (3)	O1^vii—O3—H	77.1 (11)
S—O2—O1	35.268 (17)	O2^xiv—O3—H	72.9 (11)
Fe—O2—O1	162.76 (3)	O2ⁱ—O3—H	90.6 (11)
S—O2—O2^v	35.69 (2)	O2—O3—H	116.2 (12)
Fe—O2—O2^v	103.467 (18)	O2^v—O3—H	137.8 (11)
O1—O2—O2^v	60.30 (2)	O1^xiii—O3—H	131.0 (11)
S—O2—O1^v	34.664 (18)	O1ⁱⁱⁱ—O3—H	69.9 (11)
Fe—O2—O1^v	118.93 (3)	Fe—O3—H^v	108.5 (11)
O1—O2—O1^v	59.87 (3)	Fe^v—O3—H^v	108.3 (11)
O2^v—O2—O1^v	59.554 (19)	O2^xiii—O3—H^v	23.6 (11)
S—O2—O3^ix	109.58 (3)	O2ⁱⁱⁱ—O3—H^v	118.7 (12)
Fe—O2—O3^ix	116.93 (2)	O1ⁱⁱ—O3—H^v	77.1 (11)
O1—O2—O3^ix	75.34 (2)	O1^vii—O3—H^v	146.7 (11)
O2^v—O2—O3^ix	131.04 (3)	O2^xiv—O3—H^v	90.6 (11)
O1^v—O2—O3^ix	115.35 (3)	O2ⁱ—O3—H^v	72.9 (11)
S—O2—O1ⁱⁱⁱ	161.06 (3)	O2—O3—H^v	137.8 (11)
Fe—O2—O1ⁱⁱⁱ	48.234 (17)	O2^v—O3—H^v	116.2 (12)
O1—O2—O1ⁱⁱⁱ	136.19 (2)	O1^xiii—O3—H^v	69.9 (11)
O2^v—O2—O1ⁱⁱⁱ	129.457 (18)	O1ⁱⁱⁱ—O3—H^v	131.0 (11)
O1^v—O2—O1ⁱⁱⁱ	162.93 (3)	H—O3—H^v	100 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.863 (17)	1.993 (16)	2.7537 (6)	146.4 (16)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(FeSO4H2O_N2_313K) top

Crystal data top

FeH₂Mg₀O₅S	V = 365.93 (9) Å³
M_r = 169.93	Z = 4
Monoclinic, C2/c	F(000) = 336
a = 7.0923 (10) Å	D_x = 3.084 Mg m⁻³
b = 7.5523 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.7848 (10) Å	µ = 4.58 mm⁻¹
β = 118.648 (10)°	T = 313 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.036
T_min = 0.534, T_max = 0.748	θ_max = 40.0°, θ_min = 4.2°
10474 measured reflections	h = −12→12
1139 independent reflections	k = −13→13
1115 reflections with I > 2σ(I)	l = −14→14

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.015	w = 1/[σ²(F_o²) + (0.018P)² + 0.150P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.038	(Δ/σ)_max < 0.001
S = 1.13	Δρ_max = 0.51 e Å⁻³
1139 reflections	Δρ_min = −0.71 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.209 (4)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe	0.000000	0.500000	0.000000	0.00928 (5)
S	0.000000	0.15309 (3)	0.250000	0.00781 (5)
O1	0.16949 (8)	0.04222 (8)	0.39797 (8)	0.01594 (9)
O2	0.09559 (8)	0.26774 (7)	0.15682 (8)	0.01397 (9)
O3	0.000000	0.64483 (10)	0.250000	0.01298 (11)
H	0.107 (3)	0.722 (3)	0.297 (2)	0.040 (4)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe	0.00841 (6)	0.00935 (6)	0.00991 (6)	−0.00014 (3)	0.00425 (4)	0.00092 (3)
S	0.00596 (7)	0.00716 (8)	0.00993 (8)	0.000	0.00352 (6)	0.000
O1	0.00969 (17)	0.0176 (2)	0.0190 (2)	0.00462 (16)	0.00563 (15)	0.00856 (17)
O2	0.01329 (18)	0.01247 (18)	0.0190 (2)	0.00163 (14)	0.01008 (16)	0.00557 (15)
O3	0.0133 (2)	0.0137 (3)	0.0127 (2)	0.000	0.0069 (2)	0.000

Geometric parameters (Å, º) top

Fe—O2ⁱ	2.0575 (5)	O1—O1^v	2.4035 (11)
Fe—O2	2.0575 (5)	O1—O2^v	2.4183 (8)
Fe—O1ⁱⁱ	2.1076 (6)	O1—O2^vi	2.8172 (8)
Fe—O1ⁱⁱⁱ	2.1076 (6)	O1—O3^vii	2.9734 (7)
Fe—O3	2.2325 (4)	O1—O2^viii	3.0683 (9)
Fe—O3ⁱ	2.2325 (4)	O1—O3^ix	3.1641 (7)
Fe—O2ⁱⁱ	3.4792 (7)	O1—O3^x	3.2329 (10)
Fe—O2ⁱⁱⁱ	3.4792 (7)	O1—O2^xi	3.2906 (8)
Fe—O2^iv	3.5229 (6)	O1—O2^vii	3.3632 (9)
Fe—O2^v	3.5229 (6)	O2—O2^v	2.4145 (10)
S—O1	1.4647 (5)	O2—O3^ix	2.7603 (7)
S—O1^v	1.4647 (5)	O2—O3ⁱ	2.9777 (7)
S—O2	1.4856 (5)	O2—O3	3.0932 (9)
S—O2^v	1.4856 (5)	O3—H	0.882 (18)
O1—O2	2.3992 (8)	O3—H^v	0.882 (18)

O2ⁱ—Fe—O2	180.00 (3)	O3^ix—O2—O1ⁱⁱⁱ	70.84 (2)
O2ⁱ—Fe—O1ⁱⁱ	85.11 (2)	S—O2—O3ⁱ	136.39 (3)
O2—Fe—O1ⁱⁱ	94.89 (2)	Fe—O2—O3ⁱ	48.520 (17)
O2ⁱ—Fe—O1ⁱⁱⁱ	94.89 (2)	O1—O2—O3ⁱ	147.41 (3)
O2—Fe—O1ⁱⁱⁱ	85.11 (2)	O2^v—O2—O3ⁱ	137.05 (3)
O1ⁱⁱ—Fe—O1ⁱⁱⁱ	180.0	O1^v—O2—O3ⁱ	101.96 (3)
O2ⁱ—Fe—O3	87.81 (2)	O3^ix—O2—O3ⁱ	91.842 (19)
O2—Fe—O3	92.19 (2)	O1ⁱⁱⁱ—O2—O3ⁱ	61.667 (19)
O1ⁱⁱ—Fe—O3	86.435 (18)	S—O2—O1ⁱⁱ	93.26 (3)
O1ⁱⁱⁱ—Fe—O3	93.565 (18)	Fe—O2—O1ⁱⁱ	43.189 (15)
O2ⁱ—Fe—O3ⁱ	92.19 (2)	O1—O2—O1ⁱⁱ	128.52 (3)
O2—Fe—O3ⁱ	87.81 (2)	O2^v—O2—O1ⁱⁱ	74.61 (3)
O1ⁱⁱ—Fe—O3ⁱ	93.565 (18)	O1^v—O2—O1ⁱⁱ	77.05 (3)
O1ⁱⁱⁱ—Fe—O3ⁱ	86.435 (18)	O3^ix—O2—O1ⁱⁱ	154.43 (2)
O3—Fe—O3ⁱ	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	91.38 (2)
O2ⁱ—Fe—O2ⁱⁱ	97.125 (13)	O3ⁱ—O2—O1ⁱⁱ	63.091 (18)
O2—Fe—O2ⁱⁱ	82.875 (14)	S—O2—O3	102.68 (3)
O1ⁱⁱ—Fe—O2ⁱⁱ	42.627 (18)	Fe—O2—O3	46.155 (14)
O1ⁱⁱⁱ—Fe—O2ⁱⁱ	137.373 (18)	O1—O2—O3	117.41 (3)
O3—Fe—O2ⁱⁱ	127.560 (13)	O2^v—O2—O3	67.028 (11)
O3ⁱ—Fe—O2ⁱⁱ	52.440 (13)	O1^v—O2—O3	116.78 (2)
O2ⁱ—Fe—O2ⁱⁱⁱ	82.875 (13)	O3^ix—O2—O3	124.40 (2)
O2—Fe—O2ⁱⁱⁱ	97.125 (14)	O1ⁱⁱⁱ—O2—O3	64.536 (19)
O1ⁱⁱ—Fe—O2ⁱⁱⁱ	137.373 (17)	O3ⁱ—O2—O3	94.675 (17)
O1ⁱⁱⁱ—Fe—O2ⁱⁱⁱ	42.627 (18)	O1ⁱⁱ—O2—O3	57.706 (15)
O3—Fe—O2ⁱⁱⁱ	52.440 (13)	S—O2—O1^xii	97.37 (3)
O3ⁱ—Fe—O2ⁱⁱⁱ	127.560 (13)	Fe—O2—O1^xii	110.31 (2)
O2ⁱⁱ—Fe—O2ⁱⁱⁱ	180.0	O1—O2—O1^xii	86.273 (19)
O2ⁱ—Fe—O2^iv	41.756 (18)	O2^v—O2—O1^xii	131.926 (17)
O2—Fe—O2^iv	138.244 (18)	O1^v—O2—O1^xii	74.31 (2)
O1ⁱⁱ—Fe—O2^iv	111.91 (2)	O3^ix—O2—O1^xii	58.076 (18)
O1ⁱⁱⁱ—Fe—O2^iv	68.09 (2)	O1ⁱⁱⁱ—O2—O1^xii	98.71 (2)
O3—Fe—O2^iv	119.84 (2)	O3ⁱ—O2—O1^xii	61.86 (2)
O3ⁱ—Fe—O2^iv	60.16 (2)	O1ⁱⁱ—O2—O1^xii	109.06 (2)
O2ⁱⁱ—Fe—O2^iv	95.428 (17)	O3—O2—O1^xii	156.31 (2)
O2ⁱⁱⁱ—Fe—O2^iv	84.572 (16)	S—O2—O1^vii	82.08 (3)
O2ⁱ—Fe—O2^v	138.244 (18)	Fe—O2—O1^vii	96.15 (2)
O2—Fe—O2^v	41.756 (18)	O1—O2—O1^vii	71.47 (3)
O1ⁱⁱ—Fe—O2^v	68.09 (2)	O2^v—O2—O1^vii	61.59 (2)
O1ⁱⁱⁱ—Fe—O2^v	111.91 (2)	O1^v—O2—O1^vii	116.20 (3)
O3—Fe—O2^v	60.16 (2)	O3^ix—O2—O1^vii	86.20 (2)
O3ⁱ—Fe—O2^v	119.84 (2)	O1ⁱⁱⁱ—O2—O1^vii	78.771 (18)
O2ⁱⁱ—Fe—O2^v	84.572 (17)	O3ⁱ—O2—O1^vii	138.51 (2)
O2ⁱⁱⁱ—Fe—O2^v	95.428 (16)	O1ⁱⁱ—O2—O1^vii	108.81 (2)
O2^iv—Fe—O2^v	180.000 (17)	O3—O2—O1^vii	54.649 (14)
O1—S—O1^v	110.27 (5)	O1^xii—O2—O1^vii	142.09 (2)
O1—S—O2	108.82 (3)	Fe—O3—Fe^v	121.33 (3)
O1^v—S—O2	110.11 (3)	Fe—O3—O2^xiii	111.712 (15)
O1—S—O2^v	110.11 (3)	Fe^v—O3—O2^xiii	87.683 (13)
O1^v—S—O2^v	108.82 (3)	Fe—O3—O2ⁱⁱⁱ	87.683 (14)
O2—S—O2^v	108.70 (4)	Fe^v—O3—O2ⁱⁱⁱ	111.712 (15)
S—O1—Fe^vi	136.72 (3)	O2^xiii—O3—O2ⁱⁱⁱ	140.70 (4)
S—O1—O2	35.881 (18)	Fe—O3—O1ⁱⁱ	45.029 (14)
Fe^vi—O1—O2	100.87 (3)	Fe^v—O3—O1ⁱⁱ	103.96 (3)
S—O1—O1^v	34.87 (3)	O2^xiii—O3—O1ⁱⁱ	69.932 (19)
Fe^vi—O1—O1^v	141.43 (4)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	131.505 (17)
O2—O1—O1^v	60.47 (2)	Fe—O3—O1^vii	103.96 (3)
S—O1—O2^v	35.23 (2)	Fe^v—O3—O1^vii	45.029 (14)
Fe^vi—O1—O2^v	143.43 (3)	O2^xiii—O3—O1^vii	131.505 (17)
O2—O1—O2^v	60.15 (3)	O2ⁱⁱⁱ—O3—O1^vii	69.932 (19)
O1^v—O1—O2^v	59.68 (2)	O1ⁱⁱ—O3—O1^vii	123.27 (4)
S—O1—O2^vi	128.57 (4)	Fe—O3—O2^xiv	160.16 (3)
Fe^vi—O1—O2^vi	46.693 (16)	Fe^v—O3—O2^xiv	43.667 (12)
O2—O1—O2^vi	109.09 (2)	O2^xiii—O3—O2^xiv	83.280 (18)
O1^v—O1—O2^vi	104.31 (3)	O2ⁱⁱⁱ—O3—O2^xiv	88.158 (19)
O2^v—O1—O2^vi	163.28 (3)	O1ⁱⁱ—O3—O2^xiv	139.687 (19)
S—O1—O3^vii	169.60 (4)	O1^vii—O3—O2^xiv	56.509 (18)
Fe^vi—O1—O3^vii	48.536 (13)	Fe—O3—O2ⁱ	43.667 (13)
O2—O1—O3^vii	146.97 (3)	Fe^v—O3—O2ⁱ	160.16 (3)
O1^v—O1—O3^vii	150.20 (2)	O2^xiii—O3—O2ⁱ	88.158 (19)
O2^v—O1—O3^vii	134.42 (3)	O2ⁱⁱⁱ—O3—O2ⁱ	83.281 (18)
O2^vi—O1—O3^vii	61.823 (19)	O1ⁱⁱ—O3—O2ⁱ	56.509 (18)
S—O1—O2^viii	115.32 (3)	O1^vii—O3—O2ⁱ	139.687 (19)
Fe^vi—O1—O2^viii	41.923 (16)	O2^xiv—O3—O2ⁱ	154.38 (3)
O2—O1—O2^viii	87.63 (2)	Fe—O3—O2^v	81.08 (2)
O1^v—O1—O2^viii	147.90 (2)	Fe^v—O3—O2^v	41.658 (15)
O2^v—O1—O2^viii	102.95 (3)	O2^xiii—O3—O2^v	93.112 (15)
O2^vi—O1—O2^viii	88.62 (2)	O2ⁱⁱⁱ—O3—O2^v	124.40 (2)
O3^vii—O1—O2^viii	61.57 (2)	O1ⁱⁱ—O3—O2^v	67.30 (2)
S—O1—O3^ix	92.61 (3)	O1^vii—O3—O2^v	60.73 (2)
Fe^vi—O1—O3^ix	44.766 (14)	O2^xiv—O3—O2^v	85.325 (17)
O2—O1—O3^ix	57.54 (2)	O2ⁱ—O3—O2^v	119.33 (2)
O1^v—O1—O3^ix	103.07 (3)	Fe—O3—O2	41.658 (15)
O2^v—O1—O3^ix	114.35 (3)	Fe^v—O3—O2	81.08 (2)
O2^vi—O1—O3^ix	61.96 (2)	O2^xiii—O3—O2	124.40 (2)
O3^vii—O1—O3^ix	93.30 (2)	O2ⁱⁱⁱ—O3—O2	93.112 (15)
O2^viii—O1—O3^ix	57.057 (17)	O1ⁱⁱ—O3—O2	60.73 (2)
S—O1—O3^x	103.05 (3)	O1^vii—O3—O2	67.30 (2)
Fe^vi—O1—O3^x	98.64 (2)	O2^xiv—O3—O2	119.33 (2)
O2—O1—O3^x	118.41 (3)	O2ⁱ—O3—O2	85.325 (17)
O1^v—O1—O3^x	68.178 (11)	O2^v—O3—O2	45.94 (2)
O2^v—O1—O3^x	117.78 (2)	Fe—O3—O1^xiii	120.47 (2)
O2^vi—O1—O3^x	53.758 (18)	Fe^v—O3—O1^xiii	41.669 (12)
O3^vii—O1—O3^x	83.194 (19)	O2^xiii—O3—O1^xiii	47.173 (15)
O2^viii—O1—O3^x	138.52 (2)	O2ⁱⁱⁱ—O3—O1^xiii	147.619 (17)
O3^ix—O1—O3^x	108.15 (2)	O1ⁱⁱ—O3—O1^xiii	79.915 (17)
S—O1—O2^xi	125.22 (3)	O1^vii—O3—O1^xiii	86.70 (2)
Fe^vi—O1—O2^xi	97.84 (2)	O2^xiv—O3—O1^xiii	59.852 (17)
O2—O1—O2^xi	160.91 (3)	O2ⁱ—O3—O1^xiii	127.652 (16)
O1^v—O1—O2^xi	101.96 (2)	O2^v—O3—O1^xiii	53.502 (16)
O2^v—O1—O2^xi	105.69 (2)	O2—O3—O1^xiii	98.27 (2)
O2^vi—O1—O2^xi	81.29 (2)	Fe—O3—O1ⁱⁱⁱ	41.669 (12)
O3^vii—O1—O2^xi	51.992 (16)	Fe^v—O3—O1ⁱⁱⁱ	120.47 (2)
O2^viii—O1—O2^xi	109.06 (2)	O2^xiii—O3—O1ⁱⁱⁱ	147.619 (17)
O3^ix—O1—O2^xi	139.51 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	47.173 (15)
O3^x—O1—O2^xi	54.310 (15)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	86.70 (2)
S—O1—O2^vii	112.38 (3)	O1^vii—O3—O1ⁱⁱⁱ	79.915 (17)
Fe^vi—O1—O2^vii	76.36 (2)	O2^xiv—O3—O1ⁱⁱⁱ	127.652 (16)
O2—O1—O2^vii	108.53 (3)	O2ⁱ—O3—O1ⁱⁱⁱ	59.852 (17)
O1^v—O1—O2^vii	139.60 (3)	O2^v—O3—O1ⁱⁱⁱ	98.27 (2)
O2^v—O1—O2^vii	80.81 (2)	O2—O3—O1ⁱⁱⁱ	53.502 (16)
O2^vi—O1—O2^vii	115.68 (2)	O1^xiii—O3—O1ⁱⁱⁱ	151.65 (3)
O3^vii—O1—O2^vii	58.05 (2)	Fe—O3—H	109.1 (11)
O2^viii—O1—O2^vii	43.801 (19)	Fe^v—O3—H	108.5 (11)
O3^ix—O1—O2^vii	100.56 (2)	O2^xiii—O3—H	117.7 (12)
O3^x—O1—O2^vii	132.783 (19)	O2ⁱⁱⁱ—O3—H	24.9 (11)
O2^xi—O1—O2^vii	79.523 (17)	O1ⁱⁱ—O3—H	146.8 (11)
S—O2—Fe	133.54 (3)	O1^vii—O3—H	77.7 (11)
S—O2—O1	35.298 (18)	O2^xiv—O3—H	72.4 (11)
Fe—O2—O1	162.88 (3)	O2ⁱ—O3—H	90.6 (11)
S—O2—O2^v	35.65 (2)	O2^v—O3—H	138.4 (11)
Fe—O2—O2^v	103.668 (19)	O2—O3—H	117.5 (12)
O1—O2—O2^v	60.32 (2)	O1^xiii—O3—H	130.3 (11)
S—O2—O1^v	34.663 (19)	O1ⁱⁱⁱ—O3—H	71.0 (11)
Fe—O2—O1^v	119.25 (3)	Fe—O3—H^v	108.5 (11)
O1—O2—O1^v	59.85 (3)	Fe^v—O3—H^v	109.1 (11)
O2^v—O2—O1^v	59.53 (2)	O2^xiii—O3—H^v	24.9 (11)
S—O2—O3^ix	109.61 (3)	O2ⁱⁱⁱ—O3—H^v	117.7 (12)
Fe—O2—O3^ix	116.61 (2)	O1ⁱⁱ—O3—H^v	77.7 (11)
O1—O2—O3^ix	75.29 (2)	O1^vii—O3—H^v	146.8 (11)
O2^v—O2—O3^ix	130.86 (3)	O2^xiv—O3—H^v	90.6 (11)
O1^v—O2—O3^ix	115.56 (3)	O2ⁱ—O3—H^v	72.4 (11)
S—O2—O1ⁱⁱⁱ	160.78 (3)	O2^v—O3—H^v	117.5 (12)
Fe—O2—O1ⁱⁱⁱ	48.194 (17)	O2—O3—H^v	138.4 (11)
O1—O2—O1ⁱⁱⁱ	135.86 (2)	O1^xiii—O3—H^v	71.0 (11)
O2^v—O2—O1ⁱⁱⁱ	129.364 (19)	O1ⁱⁱⁱ—O3—H^v	130.3 (11)
O1^v—O2—O1ⁱⁱⁱ	163.28 (3)	H—O3—H^v	98 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.882 (18)	1.995 (17)	2.7603 (7)	144.3 (16)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(CoSO4H2O_He_15K) top

Crystal data top

CoH₂O₅S	Z = 4
M_r = 173.01	F(000) = 340
Monoclinic, C2/c	D_x = 3.260 Mg m⁻³
a = 6.9143 (10) Å	Mo Kα radiation, λ = 0.71073 Å
b = 7.6290 (8) Å	µ = 5.34 mm⁻¹
c = 7.5815 (10) Å	T = 15 K
β = 118.191 (16)°	0.20 × 0.20 × 0.05 mm
V = 352.48 (9) Å³

Data collection top

1229 measured reflections	θ_max = 29.2°, θ_min = 4.2°
428 independent reflections	h = −9→7
383 reflections with I > 2σ(I)	k = −9→7
R_int = 0.049	l = −7→10

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.027	w = 1/[σ²(F_o²) + (0.021P)² + 0.360P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.065	(Δ/σ)_max < 0.001
S = 1.15	Δρ_max = 0.84 e Å⁻³
428 reflections	Δρ_min = −0.71 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.020 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co	0.000000	0.500000	0.000000	0.0041 (2)
S	0.000000	0.15579 (15)	0.250000	0.0042 (3)
O1	0.1722 (3)	0.0452 (3)	0.4025 (3)	0.0051 (5)
O2	0.1006 (3)	0.2687 (3)	0.1558 (3)	0.0058 (5)
O3	0.000000	0.6373 (5)	0.250000	0.0068 (7)
H	0.100 (5)	0.697 (5)	0.293 (5)	0.008 (10)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co	0.0045 (3)	0.0025 (4)	0.0049 (4)	−0.0002 (2)	0.0019 (3)	0.0002 (2)
S	0.0046 (5)	0.0026 (6)	0.0050 (5)	0.000	0.0019 (4)	0.000
O1	0.0045 (10)	0.0025 (11)	0.0079 (10)	0.0013 (9)	0.0026 (9)	0.0003 (9)
O2	0.0060 (10)	0.0034 (12)	0.0084 (10)	0.0003 (9)	0.0036 (9)	0.0019 (8)
O3	0.0042 (15)	0.0062 (18)	0.0088 (16)	0.000	0.0021 (14)	0.000

Geometric parameters (Å, º) top

Co—O2ⁱ	2.053 (2)	O1—O1^iv	2.412 (4)
Co—O2	2.053 (2)	O1—O2^iv	2.423 (3)
Co—O1ⁱⁱ	2.054 (2)	O1—O2^vi	2.787 (3)
Co—O1ⁱⁱⁱ	2.054 (2)	O1—O3^vii	2.894 (3)
Co—O3ⁱ	2.1654 (17)	O1—O2^viii	3.017 (3)
Co—O3	2.1654 (17)	O1—O3^ix	3.073 (2)
Co—O2ⁱⁱⁱ	3.440 (2)	O1—O2^x	3.251 (3)
Co—O2ⁱⁱ	3.440 (2)	O1—O2^vii	3.276 (3)
Co—O2^iv	3.482 (2)	O1—O3^xi	3.338 (4)
Co—O2^v	3.482 (2)	O2—O2^iv	2.420 (4)
S—O1	1.472 (2)	O2—O3^ix	2.698 (2)
S—O1^iv	1.472 (2)	O2—O3ⁱ	2.905 (2)
S—O2^iv	1.485 (2)	O2—O3	3.061 (4)
S—O2	1.485 (2)	O3—H	0.76 (3)
O1—O2	2.403 (3)	O3—H^iv	0.76 (3)

O2ⁱ—Co—O2	180.0	O3^ix—O2—O1ⁱⁱⁱ	74.94 (9)
O2ⁱ—Co—O1ⁱⁱ	85.48 (8)	S—O2—O3ⁱ	136.09 (12)
O2—Co—O1ⁱⁱ	94.53 (8)	Co—O2—O3ⁱ	48.10 (8)
O2ⁱ—Co—O1ⁱⁱⁱ	94.52 (8)	O1—O2—O3ⁱ	149.05 (13)
O2—Co—O1ⁱⁱⁱ	85.47 (8)	O2^iv—O2—O3ⁱ	135.12 (11)
O1ⁱⁱ—Co—O1ⁱⁱⁱ	180.0	O1^iv—O2—O3ⁱ	101.79 (10)
O2ⁱ—Co—O3ⁱ	93.00 (10)	O3^ix—O2—O3ⁱ	94.32 (7)
O2—Co—O3ⁱ	87.00 (10)	O1ⁱⁱⁱ—O2—O3ⁱ	61.07 (8)
O1ⁱⁱ—Co—O3ⁱ	93.44 (6)	S—O2—O1ⁱⁱ	92.12 (10)
O1ⁱⁱⁱ—Co—O3ⁱ	86.56 (6)	Co—O2—O1ⁱⁱ	42.75 (6)
O2ⁱ—Co—O3	87.00 (10)	O1—O2—O1ⁱⁱ	127.49 (11)
O2—Co—O3	93.00 (10)	O2^iv—O2—O1ⁱⁱ	73.17 (9)
O1ⁱⁱ—Co—O3	86.56 (6)	O1^iv—O2—O1ⁱⁱ	76.67 (9)
O1ⁱⁱⁱ—Co—O3	93.44 (6)	O3^ix—O2—O1ⁱⁱ	156.61 (9)
O3ⁱ—Co—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.02 (9)
O2ⁱ—Co—O2ⁱⁱⁱ	81.75 (3)	O3ⁱ—O2—O1ⁱⁱ	62.48 (6)
O2—Co—O2ⁱⁱⁱ	98.25 (3)	S—O2—O3	102.17 (11)
O1ⁱⁱ—Co—O2ⁱⁱⁱ	136.64 (7)	Co—O2—O3	44.95 (5)
O1ⁱⁱⁱ—Co—O2ⁱⁱⁱ	43.36 (7)	O1—O2—O3	117.12 (9)
O3ⁱ—Co—O2ⁱⁱⁱ	128.34 (5)	O2^iv—O2—O3	66.72 (5)
O3—Co—O2ⁱⁱⁱ	51.66 (5)	O1^iv—O2—O3	116.47 (9)
O2ⁱ—Co—O2ⁱⁱ	98.25 (3)	O3^ix—O2—O3	126.62 (11)
O2—Co—O2ⁱⁱ	81.75 (3)	O1ⁱⁱⁱ—O2—O3	63.19 (7)
O1ⁱⁱ—Co—O2ⁱⁱ	43.36 (7)	O3ⁱ—O2—O3	93.05 (8)
O1ⁱⁱⁱ—Co—O2ⁱⁱ	136.64 (7)	O1ⁱⁱ—O2—O3	56.86 (6)
O3ⁱ—Co—O2ⁱⁱ	51.66 (5)	S—O2—O1^xii	95.37 (12)
O3—Co—O2ⁱⁱ	128.34 (5)	Co—O2—O1^xii	113.47 (8)
O2ⁱⁱⁱ—Co—O2ⁱⁱ	180.00 (6)	O1—O2—O1^xii	84.51 (7)
O2ⁱ—Co—O2^iv	137.16 (7)	O2^iv—O2—O1^xii	129.75 (6)
O2—Co—O2^iv	42.84 (7)	O1^iv—O2—O1^xii	72.35 (9)
O1ⁱⁱ—Co—O2^iv	66.89 (7)	O3^ix—O2—O1^xii	57.32 (7)
O1ⁱⁱⁱ—Co—O2^iv	113.11 (7)	O1ⁱⁱⁱ—O2—O1^xii	102.09 (8)
O3ⁱ—Co—O2^iv	119.57 (9)	O3ⁱ—O2—O1^xii	65.39 (9)
O3—Co—O2^iv	60.43 (9)	O1ⁱⁱ—O2—O1^xii	110.40 (8)
O2ⁱⁱⁱ—Co—O2^iv	96.10 (5)	O3—O2—O1^xii	158.35 (8)
O2ⁱⁱ—Co—O2^iv	83.90 (5)	S—O2—O1^vii	82.34 (9)
O2ⁱ—Co—O2^v	42.84 (7)	Co—O2—O1^vii	94.82 (9)
O2—Co—O2^v	137.16 (7)	O1—O2—O1^vii	71.86 (9)
O1ⁱⁱ—Co—O2^v	113.11 (7)	O2^iv—O2—O1^vii	61.83 (8)
O1ⁱⁱⁱ—Co—O2^v	66.89 (7)	O1^iv—O2—O1^vii	116.57 (11)
O3ⁱ—Co—O2^v	60.43 (9)	O3^ix—O2—O1^vii	87.35 (7)
O3—Co—O2^v	119.57 (9)	O1ⁱⁱⁱ—O2—O1^vii	78.46 (7)
O2ⁱⁱⁱ—Co—O2^v	83.90 (5)	O3ⁱ—O2—O1^vii	137.30 (11)
O2ⁱⁱ—Co—O2^v	96.10 (5)	O1ⁱⁱ—O2—O1^vii	107.41 (9)
O2^iv—Co—O2^v	180.00 (7)	O3—O2—O1^vii	54.22 (5)
O1—S—O1^iv	110.05 (19)	O1^xii—O2—O1^vii	142.18 (7)
O1—S—O2^iv	110.08 (11)	Co—O3—Co^iv	122.16 (17)
O1^iv—S—O2^iv	108.75 (12)	Co—O3—O2ⁱⁱⁱ	89.33 (4)
O1—S—O2	108.75 (12)	Co^iv—O3—O2ⁱⁱⁱ	111.79 (5)
O1^iv—S—O2	110.08 (11)	Co—O3—O2^xiii	111.79 (5)
O2^iv—S—O2	109.11 (19)	Co^iv—O3—O2^xiii	89.33 (4)
S—O1—Co^vi	136.45 (14)	O2ⁱⁱⁱ—O3—O2^xiii	136.37 (17)
S—O1—O2	35.81 (7)	Co—O3—O1ⁱⁱ	45.11 (6)
Co^vi—O1—O2	100.72 (10)	Co^iv—O3—O1ⁱⁱ	103.91 (11)
S—O1—O1^iv	34.97 (10)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	133.11 (6)
Co^vi—O1—O1^iv	140.09 (15)	O2^xiii—O3—O1ⁱⁱ	70.99 (6)
O2—O1—O1^iv	60.43 (8)	Co—O3—O1^vii	103.91 (11)
S—O1—O2^iv	35.14 (7)	Co^iv—O3—O1^vii	45.11 (6)
Co^vi—O1—O2^iv	144.62 (12)	O2ⁱⁱⁱ—O3—O1^vii	70.99 (6)
O2—O1—O2^iv	60.17 (11)	O2^xiii—O3—O1^vii	133.11 (6)
O1^iv—O1—O2^iv	59.61 (8)	O1ⁱⁱ—O3—O1^vii	122.48 (15)
S—O1—O2^vi	128.08 (13)	Co—O3—O2^xiv	161.31 (13)
Co^vi—O1—O2^vi	47.25 (6)	Co^iv—O3—O2^xiv	44.90 (5)
O2—O1—O2^vi	109.75 (8)	O2ⁱⁱⁱ—O3—O2^xiv	85.69 (7)
O1^iv—O1—O2^vi	102.90 (9)	O2^xiii—O3—O2^xiv	83.78 (7)
O2^iv—O1—O2^vi	162.18 (13)	O1ⁱⁱ—O3—O2^xiv	140.86 (7)
S—O1—O3^vii	170.44 (13)	O1^vii—O3—O2^xiv	57.46 (6)
Co^vi—O1—O3^vii	48.33 (5)	Co—O3—O2ⁱ	44.90 (5)
O2—O1—O3^vii	146.59 (11)	Co^iv—O3—O2ⁱ	161.31 (13)
O1^iv—O1—O3^vii	150.10 (8)	O2ⁱⁱⁱ—O3—O2ⁱ	83.78 (7)
O2^iv—O1—O3^vii	135.38 (11)	O2^xiii—O3—O2ⁱ	85.68 (7)
O2^vi—O1—O3^vii	61.48 (7)	O1ⁱⁱ—O3—O2ⁱ	57.46 (6)
S—O1—O2^viii	114.65 (13)	O1^vii—O3—O2ⁱ	140.86 (7)
Co^vi—O1—O2^viii	42.73 (6)	O2^xiv—O3—O2ⁱ	151.40 (16)
O2—O1—O2^viii	86.62 (8)	Co—O3—O2	42.06 (7)
O1^iv—O1—O2^viii	146.95 (9)	Co^iv—O3—O2	81.61 (11)
O2^iv—O1—O2^viii	103.33 (9)	O2ⁱⁱⁱ—O3—O2	94.94 (6)
O2^vi—O1—O2^viii	89.98 (9)	O2^xiii—O3—O2	126.62 (11)
O3^vii—O1—O2^viii	62.34 (8)	O1ⁱⁱ—O3—O2	60.80 (8)
S—O1—O3^ix	92.31 (10)	O1^vii—O3—O2	66.67 (9)
Co^vi—O1—O3^ix	44.70 (5)	O2^xiv—O3—O2	120.46 (10)
O2—O1—O3^ix	57.48 (8)	O2ⁱ—O3—O2	86.95 (8)
O1^iv—O1—O3^ix	102.06 (11)	Co—O3—O2^iv	81.61 (11)
O2^iv—O1—O3^ix	114.81 (11)	Co^iv—O3—O2^iv	42.06 (7)
O2^vi—O1—O3^ix	62.76 (9)	O2ⁱⁱⁱ—O3—O2^iv	126.62 (11)
O3^vii—O1—O3^ix	93.03 (8)	O2^xiii—O3—O2^iv	94.94 (6)
O2^viii—O1—O3^ix	56.98 (6)	O1ⁱⁱ—O3—O2^iv	66.67 (9)
S—O1—O2^x	126.43 (12)	O1^vii—O3—O2^iv	60.80 (8)
Co^vi—O1—O2^x	96.53 (8)	O2^xiv—O3—O2^iv	86.95 (8)
O2—O1—O2^x	161.72 (11)	O2ⁱ—O3—O2^iv	120.46 (10)
O1^iv—O1—O2^x	102.08 (9)	O2—O3—O2^iv	46.56 (9)
O2^iv—O1—O2^x	107.65 (9)	Co—O3—O1^xiii	121.59 (11)
O2^vi—O1—O2^x	77.91 (8)	Co^iv—O3—O1^xiii	41.86 (4)
O3^vii—O1—O2^x	51.69 (6)	O2ⁱⁱⁱ—O3—O1^xiii	146.09 (6)
O2^viii—O1—O2^x	110.40 (8)	O2^xiii—O3—O1^xiii	48.69 (6)
O3^ix—O1—O2^x	137.38 (10)	O1ⁱⁱ—O3—O1^xiii	80.39 (6)
S—O1—O2^vii	111.97 (12)	O1^vii—O3—O1^xiii	86.97 (8)
Co^vi—O1—O2^vii	77.89 (7)	O2^xiv—O3—O1^xiii	60.54 (6)
O2—O1—O2^vii	108.14 (9)	O2ⁱ—O3—O1^xiii	127.21 (5)
O1^iv—O1—O2^vii	139.45 (11)	O2—O3—O1^xiii	99.63 (11)
O2^iv—O1—O2^vii	80.65 (7)	O2^iv—O3—O1^xiii	54.06 (7)
O2^vi—O1—O2^vii	117.13 (10)	Co—O3—O1ⁱⁱⁱ	41.86 (4)
O3^vii—O1—O2^vii	59.11 (8)	Co^iv—O3—O1ⁱⁱⁱ	121.59 (11)
O2^viii—O1—O2^vii	45.00 (7)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	48.69 (6)
O3^ix—O1—O2^vii	101.71 (8)	O2^xiii—O3—O1ⁱⁱⁱ	146.09 (6)
O2^x—O1—O2^vii	81.30 (5)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	86.97 (8)
S—O1—O3^xi	103.80 (11)	O1^vii—O3—O1ⁱⁱⁱ	80.39 (6)
Co^vi—O1—O3^xi	96.92 (8)	O2^xiv—O3—O1ⁱⁱⁱ	127.21 (5)
O2—O1—O3^xi	118.89 (9)	O2ⁱ—O3—O1ⁱⁱⁱ	60.54 (6)
O1^iv—O1—O3^xi	68.82 (4)	O2—O3—O1ⁱⁱⁱ	54.06 (7)
O2^iv—O1—O3^xi	118.25 (10)	O2^iv—O3—O1ⁱⁱⁱ	99.63 (11)
O2^vi—O1—O3^xi	51.31 (6)	O1^xiii—O3—O1ⁱⁱⁱ	153.58 (16)
O3^vii—O1—O3^xi	82.21 (7)	Co—O3—H	107 (3)
O2^viii—O1—O3^xi	137.87 (9)	Co^iv—O3—H	107 (3)
O3^ix—O1—O3^xi	106.77 (9)	O2ⁱⁱⁱ—O3—H	19 (3)
O2^x—O1—O3^xi	52.31 (5)	O2^xiii—O3—H	120 (3)
O2^vii—O1—O3^xi	132.74 (8)	O1ⁱⁱ—O3—H	147 (3)
S—O2—Co	131.82 (12)	O1^vii—O3—H	75 (3)
S—O2—O1	35.44 (7)	O2^xiv—O3—H	72 (3)
Co—O2—O1	161.18 (12)	O2ⁱ—O3—H	91 (3)
S—O2—O2^iv	35.45 (9)	O2—O3—H	113 (3)
Co—O2—O2^iv	101.93 (7)	O2^iv—O3—H	135 (3)
O1—O2—O2^iv	60.32 (8)	O1^xiii—O3—H	131 (3)
S—O2—O1^iv	34.77 (7)	O1ⁱⁱⁱ—O3—H	67 (3)
Co—O2—O1^iv	118.48 (10)	Co—O3—H^iv	107 (3)
O1—O2—O1^iv	59.95 (11)	Co^iv—O3—H^iv	107 (3)
O2^iv—O2—O1^iv	59.51 (8)	O2ⁱⁱⁱ—O3—H^iv	120 (3)
S—O2—O3^ix	108.09 (12)	O2^xiii—O3—H^iv	19 (3)
Co—O2—O3^ix	119.86 (10)	O1ⁱⁱ—O3—H^iv	75 (3)
O1—O2—O3^ix	73.83 (9)	O1^vii—O3—H^iv	147 (3)
O2^iv—O2—O3^ix	130.22 (11)	O2^xiv—O3—H^iv	91 (3)
O1^iv—O2—O3^ix	113.46 (13)	O2ⁱ—O3—H^iv	72 (3)
S—O2—O1ⁱⁱⁱ	160.43 (13)	O2—O3—H^iv	135 (3)
Co—O2—O1ⁱⁱⁱ	47.27 (6)	O2^iv—O3—H^iv	113 (3)
O1—O2—O1ⁱⁱⁱ	137.38 (8)	O1^xiii—O3—H^iv	67 (3)
O2^iv—O2—O1ⁱⁱⁱ	128.16 (7)	O1ⁱⁱⁱ—O3—H^iv	131 (3)
O1^iv—O2—O1ⁱⁱⁱ	162.18 (13)	H—O3—H^iv	107 (6)

O1^iv—S—O1—Co^vi	116.0 (2)	O2^iv—S—O2—Co	−38.87 (12)
O2^iv—S—O1—Co^vi	−124.15 (19)	O1^iv—S—O2—O1	−120.64 (19)
O2—S—O1—Co^vi	−4.7 (2)	O2^iv—S—O2—O1	120.09 (11)
O1^iv—S—O1—O2	120.66 (11)	O1—S—O2—O2^iv	−120.09 (11)
O2^iv—S—O1—O2	−119.48 (19)	O1^iv—S—O2—O2^iv	119.27 (12)
O2^iv—S—O1—O1^iv	119.86 (11)	O1—S—O2—O1^iv	120.64 (19)
O2—S—O1—O1^iv	−120.66 (11)	O2^iv—S—O2—O1^iv	−119.27 (12)
O1^iv—S—O1—O2^iv	−119.86 (11)	O1—S—O2—O3^ix	15.34 (16)
O2—S—O1—O2^iv	119.48 (19)	O1^iv—S—O2—O3^ix	−105.30 (13)
O1^iv—S—O1—O2^vi	51.29 (12)	O2^iv—S—O2—O3^ix	135.43 (12)
O2^iv—S—O1—O2^vi	171.15 (17)	O1—S—O2—O1ⁱⁱⁱ	−80.6 (4)
O2—S—O1—O2^vi	−69.37 (17)	O1^iv—S—O2—O1ⁱⁱⁱ	158.8 (4)
O1^iv—S—O1—O2^viii	162.34 (15)	O2^iv—S—O2—O1ⁱⁱⁱ	39.5 (3)
O2^iv—S—O1—O2^viii	−77.81 (14)	O1—S—O2—O3ⁱ	132.30 (18)
O2—S—O1—O2^viii	41.68 (15)	O1^iv—S—O2—O3ⁱ	11.7 (2)
O1^iv—S—O1—O3^ix	107.90 (10)	O2^iv—S—O2—O3ⁱ	−107.60 (19)
O2^iv—S—O1—O3^ix	−132.25 (11)	O1—S—O2—O1ⁱⁱ	−176.61 (11)
O2—S—O1—O3^ix	−12.77 (14)	O1^iv—S—O2—O1ⁱⁱ	62.75 (15)
O1^iv—S—O1—O2^x	−53.04 (10)	O2^iv—S—O2—O1ⁱⁱ	−56.52 (6)
O2^iv—S—O1—O2^x	66.81 (18)	O1—S—O2—O3	−120.09 (11)
O2—S—O1—O2^x	−173.70 (12)	O1^iv—S—O2—O3	119.27 (12)
O1^iv—S—O1—O2^vii	−148.49 (14)	O2^iv—S—O2—O3	−0.001 (1)
O2^iv—S—O1—O2^vii	−28.64 (15)	O1—S—O2—O1^xii	72.67 (11)
O2—S—O1—O2^vii	90.84 (13)	O1^iv—S—O2—O1^xii	−47.97 (14)
O1^iv—S—O1—O3^xi	−0.001 (1)	O2^iv—S—O2—O1^xii	−167.24 (9)
O2^iv—S—O1—O3^xi	119.85 (11)	O1—S—O2—O1^vii	−69.33 (13)
O2—S—O1—O3^xi	−120.66 (11)	O1^iv—S—O2—O1^vii	170.03 (11)
O1—S—O2—Co	−158.96 (15)	O2^iv—S—O2—O1^vii	50.77 (6)
O1^iv—S—O2—Co	80.4 (2)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x, y, −z+1/2; (v) x, −y+1, z−1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) x, y−1, z; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.76 (3)	1.99 (3)	2.698 (2)	154 (4)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(CoSO4H2O_He_30K) top

Crystal data top

CoH₂O₅S	Z = 4
M_r = 173.01	F(000) = 340
Monoclinic, C2/c	D_x = 3.261 Mg m⁻³
a = 6.9142 (10) Å	Mo Kα radiation, λ = 0.71073 Å
b = 7.6267 (8) Å	µ = 5.34 mm⁻¹
c = 7.581 (1) Å	T = 30 K
β = 118.179 (16)°	0.20 × 0.20 × 0.05 mm
V = 352.38 (9) Å³

Data collection top

1236 measured reflections	θ_max = 29.2°, θ_min = 4.2°
432 independent reflections	h = −7→9
386 reflections with I > 2σ(I)	k = −9→7
R_int = 0.034	l = −10→7

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.029	w = 1/[σ²(F_o²) + (0.022P)² + 0.850P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.062	(Δ/σ)_max < 0.001
S = 1.11	Δρ_max = 0.80 e Å⁻³
432 reflections	Δρ_min = −0.80 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0202 (19)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co	0.000000	0.500000	0.000000	0.0039 (2)
S	0.000000	0.15584 (15)	0.250000	0.0041 (3)
O1	0.1720 (3)	0.0451 (3)	0.4027 (3)	0.0056 (5)
O2	0.1005 (3)	0.2688 (3)	0.1559 (3)	0.0056 (5)
O3	0.000000	0.6368 (4)	0.250000	0.0056 (7)
H	0.104 (6)	0.695 (7)	0.291 (6)	0.029 (13)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co	0.0043 (3)	0.0028 (4)	0.0042 (4)	−0.0003 (2)	0.0017 (3)	0.0002 (2)
S	0.0050 (5)	0.0026 (6)	0.0052 (5)	0.000	0.0028 (4)	0.000
O1	0.0048 (10)	0.0049 (12)	0.0071 (10)	0.0006 (9)	0.0027 (9)	0.0009 (8)
O2	0.0065 (10)	0.0039 (12)	0.0069 (10)	0.0001 (9)	0.0037 (9)	0.0012 (8)
O3	0.0058 (15)	0.0043 (17)	0.0074 (15)	0.000	0.0037 (14)	0.000

Geometric parameters (Å, º) top

Co—O2ⁱ	2.052 (2)	O1—O1^v	2.411 (4)
Co—O2	2.052 (2)	O1—O2^v	2.422 (3)
Co—O1ⁱⁱ	2.056 (2)	O1—O2^vi	2.788 (3)
Co—O1ⁱⁱⁱ	2.056 (2)	O1—O3^vii	2.892 (3)
Co—O3ⁱ	2.1633 (17)	O1—O2^viii	3.018 (3)
Co—O3	2.1633 (17)	O1—O3^ix	3.074 (2)
Co—O2ⁱⁱ	3.440 (2)	O1—O2^x	3.249 (3)
Co—O2ⁱⁱⁱ	3.440 (2)	O1—O2^vii	3.273 (3)
Co—O2^iv	3.480 (2)	O1—O3^xi	3.339 (4)
Co—O2^v	3.480 (2)	O2—O2^v	2.416 (4)
S—O1^v	1.472 (2)	O2—O3^ix	2.701 (2)
S—O1	1.472 (2)	O2—O3ⁱ	2.907 (2)
S—O2	1.484 (2)	O2—O3	3.055 (4)
S—O2^v	1.484 (2)	O3—H	0.78 (4)
O1—O2	2.405 (3)	O3—H^v	0.78 (4)

O2ⁱ—Co—O2	180.0	O3^ix—O2—O1ⁱⁱⁱ	74.94 (9)
O2ⁱ—Co—O1ⁱⁱ	85.46 (8)	S—O2—O3ⁱ	136.09 (12)
O2—Co—O1ⁱⁱ	94.54 (8)	Co—O2—O3ⁱ	48.01 (7)
O2ⁱ—Co—O1ⁱⁱⁱ	94.54 (8)	O1—O2—O3ⁱ	149.07 (12)
O2—Co—O1ⁱⁱⁱ	85.46 (8)	O2^v—O2—O3ⁱ	135.10 (12)
O1ⁱⁱ—Co—O1ⁱⁱⁱ	180.00 (13)	O1^v—O2—O3ⁱ	101.77 (10)
O2ⁱ—Co—O3ⁱ	92.85 (10)	O3^ix—O2—O3ⁱ	94.32 (7)
O2—Co—O3ⁱ	87.15 (10)	O1ⁱⁱⁱ—O2—O3ⁱ	60.99 (8)
O1ⁱⁱ—Co—O3ⁱ	93.51 (6)	S—O2—O1ⁱⁱ	92.12 (10)
O1ⁱⁱⁱ—Co—O3ⁱ	86.49 (6)	Co—O2—O1ⁱⁱ	42.78 (6)
O2ⁱ—Co—O3	87.15 (10)	O1—O2—O1ⁱⁱ	127.44 (12)
O2—Co—O3	92.85 (10)	O2^v—O2—O1ⁱⁱ	73.14 (9)
O1ⁱⁱ—Co—O3	86.49 (6)	O1^v—O2—O1ⁱⁱ	76.68 (9)
O1ⁱⁱⁱ—Co—O3	93.51 (6)	O3^ix—O2—O1ⁱⁱ	156.64 (9)
O3ⁱ—Co—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.10 (9)
O2ⁱ—Co—O2ⁱⁱ	98.22 (3)	O3ⁱ—O2—O1ⁱⁱ	62.48 (6)
O2—Co—O2ⁱⁱ	81.78 (3)	S—O2—O3	102.21 (11)
O1ⁱⁱ—Co—O2ⁱⁱ	43.39 (7)	Co—O2—O3	45.01 (5)
O1ⁱⁱⁱ—Co—O2ⁱⁱ	136.61 (7)	O1—O2—O3	117.13 (9)
O3ⁱ—Co—O2ⁱⁱ	51.72 (5)	O2^v—O2—O3	66.71 (5)
O3—Co—O2ⁱⁱ	128.28 (5)	O1^v—O2—O3	116.54 (9)
O2ⁱ—Co—O2ⁱⁱⁱ	81.78 (3)	O3^ix—O2—O3	126.73 (11)
O2—Co—O2ⁱⁱⁱ	98.22 (3)	O1ⁱⁱⁱ—O2—O3	63.30 (7)
O1ⁱⁱ—Co—O2ⁱⁱⁱ	136.61 (7)	O3ⁱ—O2—O3	93.02 (7)
O1ⁱⁱⁱ—Co—O2ⁱⁱⁱ	43.39 (7)	O1ⁱⁱ—O2—O3	56.87 (6)
O3ⁱ—Co—O2ⁱⁱⁱ	128.28 (5)	S—O2—O1^xii	95.30 (11)
O3—Co—O2ⁱⁱⁱ	51.72 (5)	Co—O2—O1^xii	113.41 (8)
O2ⁱⁱ—Co—O2ⁱⁱⁱ	180.0	O1—O2—O1^xii	84.49 (7)
O2ⁱ—Co—O2^iv	42.79 (8)	O2^v—O2—O1^xii	129.73 (6)
O2—Co—O2^iv	137.21 (8)	O1^v—O2—O1^xii	72.22 (9)
O1ⁱⁱ—Co—O2^iv	113.12 (7)	O3^ix—O2—O1^xii	57.27 (7)
O1ⁱⁱⁱ—Co—O2^iv	66.88 (7)	O1ⁱⁱⁱ—O2—O1^xii	102.01 (8)
O3ⁱ—Co—O2^iv	60.32 (9)	O3ⁱ—O2—O1^xii	65.42 (8)
O3—Co—O2^iv	119.68 (9)	O1ⁱⁱ—O2—O1^xii	110.37 (8)
O2ⁱⁱ—Co—O2^iv	96.12 (5)	O3—O2—O1^xii	158.36 (8)
O2ⁱⁱⁱ—Co—O2^iv	83.88 (5)	S—O2—O1^vii	82.44 (9)
O2ⁱ—Co—O2^v	137.21 (8)	Co—O2—O1^vii	94.87 (9)
O2—Co—O2^v	42.79 (8)	O1—O2—O1^vii	71.90 (9)
O1ⁱⁱ—Co—O2^v	66.88 (7)	O2^v—O2—O1^vii	61.91 (8)
O1ⁱⁱⁱ—Co—O2^v	113.12 (7)	O1^v—O2—O1^vii	116.71 (11)
O3ⁱ—Co—O2^v	119.68 (9)	O3^ix—O2—O1^vii	87.35 (7)
O3—Co—O2^v	60.32 (9)	O1ⁱⁱⁱ—O2—O1^vii	78.48 (6)
O2ⁱⁱ—Co—O2^v	83.88 (5)	O3ⁱ—O2—O1^vii	137.23 (10)
O2ⁱⁱⁱ—Co—O2^v	96.12 (5)	O1ⁱⁱ—O2—O1^vii	107.47 (9)
O2^iv—Co—O2^v	180.00 (4)	O3—O2—O1^vii	54.24 (5)
O1^v—S—O1	109.97 (19)	O1^xii—O2—O1^vii	142.15 (8)
O1^v—S—O2	110.06 (11)	Co—O3—Co^v	122.35 (16)
O1—S—O2	108.87 (12)	Co—O3—O2^xiii	111.82 (5)
O1^v—S—O2^v	108.87 (12)	Co^v—O3—O2^xiii	89.32 (5)
O1—S—O2^v	110.06 (11)	Co—O3—O2ⁱⁱⁱ	89.32 (5)
O2—S—O2^v	109.00 (18)	Co^v—O3—O2ⁱⁱⁱ	111.82 (5)
S—O1—Co^vi	136.29 (14)	O2^xiii—O3—O2ⁱⁱⁱ	136.20 (17)
S—O1—O2	35.73 (7)	Co—O3—O1ⁱⁱ	45.21 (5)
Co^vi—O1—O2	100.64 (10)	Co^v—O3—O1ⁱⁱ	104.00 (11)
S—O1—O1^v	35.01 (9)	O2^xiii—O3—O1ⁱⁱ	70.96 (6)
Co^vi—O1—O1^v	139.94 (15)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	133.16 (6)
O2—O1—O1^v	60.40 (8)	Co—O3—O1^vii	104.00 (11)
S—O1—O2^v	35.14 (7)	Co^v—O3—O1^vii	45.21 (5)
Co^vi—O1—O2^v	144.52 (12)	O2^xiii—O3—O1^vii	133.16 (6)
O2—O1—O2^v	60.08 (11)	O2ⁱⁱⁱ—O3—O1^vii	70.96 (6)
O1^v—O1—O2^v	59.67 (8)	O1ⁱⁱ—O3—O1^vii	122.67 (15)
S—O1—O2^vi	127.99 (12)	Co—O3—O2^xiv	161.42 (12)
Co^vi—O1—O2^vi	47.22 (6)	Co^v—O3—O2^xiv	44.84 (5)
O2—O1—O2^vi	109.67 (8)	O2^xiii—O3—O2^xiv	83.72 (7)
O1^v—O1—O2^vi	102.83 (9)	O2ⁱⁱⁱ—O3—O2^xiv	85.68 (7)
O2^v—O1—O2^vi	162.13 (13)	O1ⁱⁱ—O3—O2^xiv	140.84 (7)
S—O1—O3^vii	170.47 (14)	O1^vii—O3—O2^xiv	57.47 (6)
Co^vi—O1—O3^vii	48.31 (5)	Co—O3—O2ⁱ	44.84 (5)
O2—O1—O3^vii	146.46 (11)	Co^v—O3—O2ⁱ	161.42 (12)
O1^v—O1—O3^vii	150.24 (8)	O2^xiii—O3—O2ⁱ	85.68 (7)
O2^v—O1—O3^vii	135.44 (11)	O2ⁱⁱⁱ—O3—O2ⁱ	83.72 (7)
O2^vi—O1—O3^vii	61.54 (7)	O1ⁱⁱ—O3—O2ⁱ	57.47 (6)
S—O1—O2^viii	114.60 (13)	O1^vii—O3—O2ⁱ	140.84 (7)
Co^vi—O1—O2^viii	42.69 (6)	O2^xiv—O3—O2ⁱ	151.33 (16)
O2—O1—O2^viii	86.59 (8)	Co—O3—O2	42.14 (7)
O1^v—O1—O2^viii	146.90 (9)	Co^v—O3—O2	81.71 (11)
O2^v—O1—O2^viii	103.32 (9)	O2^xiii—O3—O2	126.72 (11)
O2^vi—O1—O2^viii	89.90 (9)	O2ⁱⁱⁱ—O3—O2	95.00 (6)
O3^vii—O1—O2^viii	62.22 (8)	O1ⁱⁱ—O3—O2	60.91 (8)
S—O1—O3^ix	92.24 (10)	O1^vii—O3—O2	66.73 (9)
Co^vi—O1—O3^ix	44.62 (5)	O2^xiv—O3—O2	120.50 (10)
O2—O1—O3^ix	57.51 (8)	O2ⁱ—O3—O2	86.98 (7)
O1^v—O1—O3^ix	101.95 (11)	Co—O3—O2^v	81.71 (11)
O2^v—O1—O3^ix	114.77 (11)	Co^v—O3—O2^v	42.14 (7)
O2^vi—O1—O3^ix	62.60 (9)	O2^xiii—O3—O2^v	95.00 (6)
O3^vii—O1—O3^ix	92.92 (8)	O2ⁱⁱⁱ—O3—O2^v	126.73 (11)
O2^viii—O1—O3^ix	56.99 (6)	O1ⁱⁱ—O3—O2^v	66.73 (9)
S—O1—O2^x	126.55 (12)	O1^vii—O3—O2^v	60.91 (8)
Co^vi—O1—O2^x	96.57 (8)	O2^xiv—O3—O2^v	86.98 (7)
O2—O1—O2^x	161.77 (12)	O2ⁱ—O3—O2^v	120.50 (10)
O1^v—O1—O2^x	102.18 (9)	O2—O3—O2^v	46.59 (9)
O2^v—O1—O2^x	107.78 (9)	Co—O3—O1^xiii	121.69 (11)
O2^vi—O1—O2^x	77.99 (8)	Co^v—O3—O1^xiii	41.87 (4)
O3^vii—O1—O2^x	51.77 (6)	O2^xiii—O3—O1^xiii	48.69 (6)
O2^viii—O1—O2^x	110.37 (8)	O2ⁱⁱⁱ—O3—O1^xiii	146.08 (6)
O3^ix—O1—O2^x	137.31 (10)	O1ⁱⁱ—O3—O1^xiii	80.38 (6)
S—O1—O2^vii	112.02 (12)	O1^vii—O3—O1^xiii	87.08 (8)
Co^vi—O1—O2^vii	77.84 (7)	O2^xiv—O3—O1^xiii	60.52 (6)
O2—O1—O2^vii	108.10 (9)	O2ⁱ—O3—O1^xiii	127.21 (6)
O1^v—O1—O2^vii	139.59 (11)	O2—O3—O1^xiii	99.71 (11)
O2^v—O1—O2^vii	80.72 (7)	O2^v—O3—O1^xiii	54.10 (7)
O2^vi—O1—O2^vii	117.10 (10)	Co—O3—O1ⁱⁱⁱ	41.87 (4)
O3^vii—O1—O2^vii	59.02 (8)	Co^v—O3—O1ⁱⁱⁱ	121.69 (11)
O2^viii—O1—O2^vii	44.95 (8)	O2^xiii—O3—O1ⁱⁱⁱ	146.08 (6)
O3^ix—O1—O2^vii	101.68 (8)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	48.68 (6)
O2^x—O1—O2^vii	81.32 (5)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	87.08 (8)
S—O1—O3^xi	103.85 (11)	O1^vii—O3—O1ⁱⁱⁱ	80.38 (6)
Co^vi—O1—O3^xi	96.91 (8)	O2^xiv—O3—O1ⁱⁱⁱ	127.21 (6)
O2—O1—O3^xi	118.91 (9)	O2ⁱ—O3—O1ⁱⁱⁱ	60.52 (6)
O1^v—O1—O3^xi	68.84 (4)	O2—O3—O1ⁱⁱⁱ	54.10 (7)
O2^v—O1—O3^xi	118.34 (9)	O2^v—O3—O1ⁱⁱⁱ	99.71 (11)
O2^vi—O1—O3^xi	51.34 (6)	O1^xiii—O3—O1ⁱⁱⁱ	153.71 (15)
O3^vii—O1—O3^xi	82.30 (7)	Co—O3—H	104 (3)
O2^viii—O1—O3^xi	137.81 (9)	Co^v—O3—H	108 (3)
O3^ix—O1—O3^xi	106.67 (9)	O2^xiii—O3—H	122 (4)
O2^x—O1—O3^xi	52.34 (5)	O2ⁱⁱⁱ—O3—H	16 (3)
O2^vii—O1—O3^xi	132.77 (8)	O1ⁱⁱ—O3—H	145 (3)
S—O2—Co	131.88 (13)	O1^vii—O3—H	74 (3)
S—O2—O1	35.40 (7)	O2^xiv—O3—H	74 (3)
Co—O2—O1	161.24 (12)	O2ⁱ—O3—H	90 (3)
S—O2—O2^v	35.50 (9)	O2—O3—H	110 (4)
Co—O2—O2^v	101.97 (8)	O2^v—O3—H	135 (3)
O1—O2—O2^v	60.32 (8)	O1^xiii—O3—H	134 (3)
S—O2—O1^v	34.81 (7)	O1ⁱⁱⁱ—O3—H	64 (3)
Co—O2—O1^v	118.50 (10)	Co—O3—H^v	108 (3)
O1—O2—O1^v	59.93 (11)	Co^v—O3—H^v	104 (3)
O2^v—O2—O1^v	59.60 (8)	O2^xiii—O3—H^v	16 (3)
S—O2—O3^ix	108.00 (12)	O2ⁱⁱⁱ—O3—H^v	122 (4)
Co—O2—O3^ix	119.90 (11)	O1ⁱⁱ—O3—H^v	74 (3)
O1—O2—O3^ix	73.80 (9)	O1^vii—O3—H^v	145 (3)
O2^v—O2—O3^ix	130.22 (11)	O2^xiv—O3—H^v	90 (3)
O1^v—O2—O3^ix	113.30 (12)	O2ⁱ—O3—H^v	74 (3)
S—O2—O1ⁱⁱⁱ	160.56 (13)	O2—O3—H^v	135 (3)
Co—O2—O1ⁱⁱⁱ	47.32 (6)	O2^v—O3—H^v	110 (4)
O1—O2—O1ⁱⁱⁱ	137.40 (8)	O1^xiii—O3—H^v	64 (3)
O2^v—O2—O1ⁱⁱⁱ	128.26 (7)	O1ⁱⁱⁱ—O3—H^v	134 (3)
O1^v—O2—O1ⁱⁱⁱ	162.13 (13)	H—O3—H^v	110 (7)

O1^v—S—O1—Co^vi	115.9 (2)	O2^v—S—O2—Co	−38.96 (12)
O2—S—O1—Co^vi	−4.7 (2)	O1^v—S—O2—O1	−120.60 (19)
O2^v—S—O1—Co^vi	−124.14 (19)	O2^v—S—O2—O1	120.07 (11)
O1^v—S—O1—O2	120.66 (11)	O1^v—S—O2—O2^v	119.33 (11)
O2^v—S—O1—O2	−119.41 (19)	O1—S—O2—O2^v	−120.07 (11)
O2—S—O1—O1^v	−120.66 (11)	O1—S—O2—O1^v	120.60 (19)
O2^v—S—O1—O1^v	119.94 (11)	O2^v—S—O2—O1^v	−119.33 (11)
O1^v—S—O1—O2^v	−119.94 (11)	O1^v—S—O2—O3^ix	−105.14 (13)
O2—S—O1—O2^v	119.41 (19)	O1—S—O2—O3^ix	15.46 (15)
O1^v—S—O1—O2^vi	51.41 (12)	O2^v—S—O2—O3^ix	135.53 (12)
O2—S—O1—O2^vi	−69.25 (17)	O1^v—S—O2—O1ⁱⁱⁱ	159.1 (4)
O2^v—S—O1—O2^vi	171.35 (17)	O1—S—O2—O1ⁱⁱⁱ	−80.3 (4)
O1^v—S—O1—O2^viii	162.21 (15)	O2^v—S—O2—O1ⁱⁱⁱ	39.8 (4)
O2—S—O1—O2^viii	41.56 (14)	O1^v—S—O2—O3ⁱ	11.7 (2)
O2^v—S—O1—O2^viii	−77.85 (15)	O1—S—O2—O3ⁱ	132.33 (18)
O1^v—S—O1—O3^ix	107.78 (10)	O2^v—S—O2—O3ⁱ	−107.61 (19)
O2—S—O1—O3^ix	−12.88 (13)	O1^v—S—O2—O1ⁱⁱ	62.81 (14)
O2^v—S—O1—O3^ix	−132.29 (11)	O1—S—O2—O1ⁱⁱ	−176.59 (11)
O1^v—S—O1—O2^x	−53.09 (10)	O2^v—S—O2—O1ⁱⁱ	−56.52 (6)
O2—S—O1—O2^x	−173.75 (13)	O1^v—S—O2—O3	119.33 (11)
O2^v—S—O1—O2^x	66.85 (18)	O1—S—O2—O3	−120.07 (11)
O1^v—S—O1—O2^vii	−148.67 (14)	O2^v—S—O2—O3	0.000 (1)
O2—S—O1—O2^vii	90.67 (13)	O1^v—S—O2—O1^xii	−47.88 (14)
O2^v—S—O1—O2^vii	−28.73 (15)	O1—S—O2—O1^xii	72.72 (11)
O1^v—S—O1—O3^xi	0.000 (1)	O2^v—S—O2—O1^xii	−167.21 (10)
O2—S—O1—O3^xi	−120.66 (11)	O1^v—S—O2—O1^vii	170.15 (11)
O2^v—S—O1—O3^xi	119.94 (11)	O1—S—O2—O1^vii	−69.25 (13)
O1^v—S—O2—Co	80.37 (19)	O2^v—S—O2—O1^vii	50.82 (6)
O1—S—O2—Co	−159.03 (15)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x, −y+1, z−1/2; (v) −x, y, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) x, y−1, z; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.78 (4)	1.97 (4)	2.701 (2)	158 (5)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(CoSO4H2O_N2_113K) top

Crystal data top

CoH₂O₅S	V = 353.01 (9) Å³
M_r = 173.01	Z = 4
Monoclinic, C2/c	F(000) = 340
a = 6.9295 (10) Å	D_x = 3.255 Mg m⁻³
b = 7.6205 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.5982 (10) Å	µ = 5.33 mm⁻¹
β = 118.381 (10)°	T = 113 K

Data collection top

10503 measured reflections	θ_max = 40.0°, θ_min = 4.2°
1095 independent reflections	h = −12→12
1086 reflections with I > 2σ(I)	k = −13→13
R_int = 0.019	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.012	w = 1/[σ²(F_o²) + (0.010P)² + 0.320P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.028	(Δ/σ)_max < 0.001
S = 1.15	Δρ_max = 0.50 e Å⁻³
1095 reflections	Δρ_min = −0.43 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0218 (8)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co	0.000000	0.500000	0.000000	0.00327 (3)
S	0.000000	0.15532 (2)	0.250000	0.00313 (4)
O1	0.17207 (7)	0.04480 (6)	0.40193 (7)	0.00652 (7)
O2	0.09983 (7)	0.26818 (6)	0.15527 (7)	0.00564 (7)
O3	0.000000	0.63777 (8)	0.250000	0.00535 (9)
H	0.110 (2)	0.704 (2)	0.294 (2)	0.022 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co	0.00299 (5)	0.00348 (5)	0.00344 (5)	−0.00003 (3)	0.00161 (3)	0.00024 (3)
S	0.00255 (7)	0.00322 (7)	0.00371 (7)	0.000	0.00155 (5)	0.000
O1	0.00425 (14)	0.00740 (16)	0.00727 (16)	0.00203 (12)	0.00220 (13)	0.00341 (13)
O2	0.00567 (15)	0.00528 (15)	0.00750 (16)	0.00047 (12)	0.00437 (13)	0.00230 (12)
O3	0.0051 (2)	0.0057 (2)	0.0055 (2)	0.000	0.00273 (17)	0.000

Geometric parameters (Å, º) top

Co—O2	2.0531 (5)	O1—O1^iv	2.4048 (10)
Co—O2ⁱ	2.0531 (5)	O1—O2^iv	2.4203 (7)
Co—O1ⁱⁱ	2.0557 (5)	O1—O2^vi	2.7900 (7)
Co—O1ⁱⁱⁱ	2.0557 (5)	O1—O3^vii	2.8950 (7)
Co—O3	2.1704 (4)	O1—O2^viii	3.0164 (8)
Co—O3ⁱ	2.1704 (4)	O1—O3^ix	3.0809 (6)
Co—O2ⁱⁱⁱ	3.4383 (6)	O1—O2^x	3.2498 (7)
Co—O2ⁱⁱ	3.4383 (6)	O1—O2^vii	3.2854 (8)
Co—O2^iv	3.4903 (6)	O1—O3^xi	3.3267 (9)
Co—O2^v	3.4903 (6)	O2—O2^iv	2.4248 (9)
S—O1^iv	1.4680 (5)	O2—O3^ix	2.7014 (6)
S—O1	1.4680 (5)	O2—O3ⁱ	2.9068 (6)
S—O2^iv	1.4865 (5)	O2—O3	3.0663 (8)
S—O2	1.4865 (5)	O3—H	0.839 (15)
O1—O2	2.4018 (7)	O3—H^iv	0.839 (15)

O2—Co—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	74.55 (2)
O2—Co—O1ⁱⁱ	94.47 (2)	S—O2—O3ⁱ	136.42 (3)
O2ⁱ—Co—O1ⁱⁱ	85.53 (2)	Co—O2—O3ⁱ	48.210 (15)
O2—Co—O1ⁱⁱⁱ	85.53 (2)	O1—O2—O3ⁱ	149.06 (3)
O2ⁱ—Co—O1ⁱⁱⁱ	94.47 (2)	O1^iv—O2—O3ⁱ	102.14 (2)
O1ⁱⁱ—Co—O1ⁱⁱⁱ	180.0	O2^iv—O2—O3ⁱ	135.50 (3)
O2—Co—O3	93.06 (2)	O3^ix—O2—O3ⁱ	94.026 (18)
O2ⁱ—Co—O3	86.94 (2)	O1ⁱⁱⁱ—O2—O3ⁱ	61.044 (17)
O1ⁱⁱ—Co—O3	86.430 (16)	S—O2—O1ⁱⁱ	92.30 (2)
O1ⁱⁱⁱ—Co—O3	93.570 (16)	Co—O2—O1ⁱⁱ	42.800 (13)
O2—Co—O3ⁱ	86.94 (2)	O1—O2—O1ⁱⁱ	127.59 (3)
O2ⁱ—Co—O3ⁱ	93.06 (2)	O1^iv—O2—O1ⁱⁱ	76.87 (2)
O1ⁱⁱ—Co—O3ⁱ	93.570 (16)	O2^iv—O2—O1ⁱⁱ	73.38 (2)
O1ⁱⁱⁱ—Co—O3ⁱ	86.430 (16)	O3^ix—O2—O1ⁱⁱ	156.45 (2)
O3—Co—O3ⁱ	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.07 (2)
O2—Co—O2ⁱⁱⁱ	98.293 (13)	O3ⁱ—O2—O1ⁱⁱ	62.652 (16)
O2ⁱ—Co—O2ⁱⁱⁱ	81.707 (13)	S—O2—O3	102.06 (2)
O1ⁱⁱ—Co—O2ⁱⁱⁱ	136.648 (16)	Co—O2—O3	44.975 (12)
O1ⁱⁱⁱ—Co—O2ⁱⁱⁱ	43.352 (16)	O1—O2—O3	117.03 (2)
O3—Co—O2ⁱⁱⁱ	51.775 (12)	O1^iv—O2—O3	116.42 (2)
O3ⁱ—Co—O2ⁱⁱⁱ	128.225 (13)	O2^iv—O2—O3	66.710 (10)
O2—Co—O2ⁱⁱ	81.707 (12)	O3^ix—O2—O3	126.36 (2)
O2ⁱ—Co—O2ⁱⁱ	98.293 (13)	O1ⁱⁱⁱ—O2—O3	63.276 (17)
O1ⁱⁱ—Co—O2ⁱⁱ	43.352 (16)	O3ⁱ—O2—O3	93.185 (16)
O1ⁱⁱⁱ—Co—O2ⁱⁱ	136.648 (16)	O1ⁱⁱ—O2—O3	56.833 (13)
O3—Co—O2ⁱⁱ	128.224 (12)	S—O2—O1^xii	95.76 (2)
O3ⁱ—Co—O2ⁱⁱ	51.776 (12)	Co—O2—O1^xii	113.32 (2)
O2ⁱⁱⁱ—Co—O2ⁱⁱ	180.0	O1—O2—O1^xii	84.744 (17)
O2—Co—O2^iv	42.786 (17)	O1^iv—O2—O1^xii	72.75 (2)
O2ⁱ—Co—O2^iv	137.215 (17)	O2^iv—O2—O1^xii	130.066 (14)
O1ⁱⁱ—Co—O2^iv	66.967 (18)	O3^ix—O2—O1^xii	57.330 (16)
O1ⁱⁱⁱ—Co—O2^iv	113.032 (18)	O1ⁱⁱⁱ—O2—O1^xii	101.774 (19)
O3—Co—O2^iv	60.368 (19)	O3ⁱ—O2—O1^xii	65.136 (19)
O3ⁱ—Co—O2^iv	119.631 (18)	O1ⁱⁱ—O2—O1^xii	110.49 (2)
O2ⁱⁱⁱ—Co—O2^iv	96.022 (15)	O3—O2—O1^xii	158.221 (18)
O2ⁱⁱ—Co—O2^iv	83.978 (15)	S—O2—O1^vii	82.14 (2)
O2—Co—O2^v	137.214 (17)	Co—O2—O1^vii	94.70 (2)
O2ⁱ—Co—O2^v	42.785 (17)	O1—O2—O1^vii	71.82 (2)
O1ⁱⁱ—Co—O2^v	113.033 (18)	O1^iv—O2—O1^vii	116.33 (2)
O1ⁱⁱⁱ—Co—O2^v	66.968 (18)	O2^iv—O2—O1^vii	61.61 (2)
O3—Co—O2^v	119.632 (19)	O3^ix—O2—O1^vii	87.332 (19)
O3ⁱ—Co—O2^v	60.369 (18)	O1ⁱⁱⁱ—O2—O1^vii	78.425 (16)
O2ⁱⁱⁱ—Co—O2^v	83.978 (15)	O3ⁱ—O2—O1^vii	137.25 (2)
O2ⁱⁱ—Co—O2^v	96.022 (15)	O1ⁱⁱ—O2—O1^vii	107.28 (2)
O2^iv—Co—O2^v	180.000 (13)	O3—O2—O1^vii	54.096 (12)
O1^iv—S—O1	109.98 (4)	O1^xii—O2—O1^vii	142.222 (18)
O1^iv—S—O2^iv	108.77 (3)	Co—O3—Co^iv	122.14 (3)
O1—S—O2^iv	110.01 (3)	Co—O3—O2ⁱⁱⁱ	89.090 (13)
O1^iv—S—O2	110.01 (3)	Co^iv—O3—O2ⁱⁱⁱ	111.826 (14)
O1—S—O2	108.77 (3)	Co—O3—O2^xiii	111.827 (14)
O2^iv—S—O2	109.30 (4)	Co^iv—O3—O2^xiii	89.089 (13)
S—O1—Co^vi	136.47 (3)	O2ⁱⁱⁱ—O3—O2^xiii	136.83 (3)
S—O1—O2	35.873 (16)	Co—O3—O1ⁱⁱ	45.131 (13)
Co^vi—O1—O2	100.66 (2)	Co^iv—O3—O1ⁱⁱ	103.92 (2)
S—O1—O1^iv	35.01 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	132.906 (16)
Co^vi—O1—O1^iv	140.25 (3)	O2^xiii—O3—O1ⁱⁱ	70.901 (17)
O2—O1—O1^iv	60.469 (19)	Co—O3—O1^vii	103.92 (2)
S—O1—O2^iv	35.246 (17)	Co^iv—O3—O1^vii	45.131 (13)
Co^vi—O1—O2^iv	144.48 (3)	O2ⁱⁱⁱ—O3—O1^vii	70.901 (16)
O2—O1—O2^iv	60.37 (2)	O2^xiii—O3—O1^vii	132.905 (15)
O1^iv—O1—O2^iv	59.705 (19)	O1ⁱⁱ—O3—O1^vii	122.55 (3)
S—O1—O2^vi	128.28 (3)	Co—O3—O2^xiv	161.34 (2)
Co^vi—O1—O2^vi	47.194 (14)	Co^iv—O3—O2^xiv	44.854 (12)
O2—O1—O2^vi	109.71 (2)	O2ⁱⁱⁱ—O3—O2^xiv	85.974 (18)
O1^iv—O1—O2^vi	103.13 (2)	O2^xiii—O3—O2^xiv	83.615 (18)
O2^iv—O1—O2^vi	162.50 (3)	O1ⁱⁱ—O3—O2^xiv	140.759 (16)
S—O1—O3^vii	170.25 (3)	O1^vii—O3—O2^xiv	57.486 (15)
Co^vi—O1—O3^vii	48.439 (12)	Co—O3—O2ⁱ	44.854 (12)
O2—O1—O3^vii	146.66 (2)	Co^iv—O3—O2ⁱ	161.34 (2)
O1^iv—O1—O3^vii	150.070 (17)	O2ⁱⁱⁱ—O3—O2ⁱ	83.616 (17)
O2^iv—O1—O3^vii	135.08 (2)	O2^xiii—O3—O2ⁱ	85.974 (18)
O2^vi—O1—O3^vii	61.470 (17)	O1ⁱⁱ—O3—O2ⁱ	57.486 (15)
S—O1—O2^viii	114.53 (3)	O1^vii—O3—O2ⁱ	140.759 (16)
Co^vi—O1—O2^viii	42.735 (14)	O2^xiv—O3—O2ⁱ	151.45 (3)
O2—O1—O2^viii	86.57 (2)	Co—O3—O2^iv	81.66 (2)
O1^iv—O1—O2^viii	146.921 (19)	Co^iv—O3—O2^iv	41.961 (14)
O2^iv—O1—O2^viii	103.13 (2)	O2ⁱⁱⁱ—O3—O2^iv	126.36 (2)
O2^vi—O1—O2^viii	89.93 (2)	O2^xiii—O3—O2^iv	94.756 (14)
O3^vii—O1—O2^viii	62.453 (19)	O1ⁱⁱ—O3—O2^iv	66.817 (19)
S—O1—O3^ix	92.38 (2)	O1^vii—O3—O2^iv	60.714 (18)
Co^vi—O1—O3^ix	44.676 (13)	O2^xiv—O3—O2^iv	86.816 (16)
O2—O1—O3^ix	57.449 (18)	O2ⁱ—O3—O2^iv	120.56 (2)
O1^iv—O1—O3^ix	102.22 (3)	Co—O3—O2	41.961 (14)
O2^iv—O1—O3^ix	114.89 (2)	Co^iv—O3—O2	81.66 (2)
O2^vi—O1—O3^ix	62.741 (19)	O2ⁱⁱⁱ—O3—O2	94.756 (14)
O3^vii—O1—O3^ix	93.115 (18)	O2^xiii—O3—O2	126.36 (2)
O2^viii—O1—O3^ix	56.933 (16)	O1ⁱⁱ—O3—O2	60.714 (18)
S—O1—O2^x	126.20 (3)	O1^vii—O3—O2	66.817 (19)
Co^vi—O1—O2^x	96.798 (19)	O2^xiv—O3—O2	120.56 (2)
O2—O1—O2^x	161.57 (3)	O2ⁱ—O3—O2	86.815 (16)
O1^iv—O1—O2^x	101.95 (2)	O2^iv—O3—O2	46.58 (2)
O2^iv—O1—O2^x	107.25 (2)	Co—O3—O1^xiii	121.57 (2)
O2^vi—O1—O2^x	78.226 (19)	Co^iv—O3—O1^xiii	41.755 (11)
O3^vii—O1—O2^x	51.769 (15)	O2ⁱⁱⁱ—O3—O1^xiii	146.231 (16)
O2^viii—O1—O2^x	110.49 (2)	O2^xiii—O3—O1^xiii	48.540 (14)
O3^ix—O1—O2^x	137.68 (2)	O1ⁱⁱ—O3—O1^xiii	80.404 (16)
S—O1—O2^vii	111.84 (3)	O1^vii—O3—O1^xiii	86.886 (18)
Co^vi—O1—O2^vii	77.875 (19)	O2^xiv—O3—O1^xiii	60.415 (15)
O2—O1—O2^vii	108.18 (2)	O2ⁱ—O3—O1^xiii	127.381 (15)
O1^iv—O1—O2^vii	139.29 (2)	O2^iv—O3—O1^xiii	53.983 (14)
O2^iv—O1—O2^vii	80.406 (19)	O2—O3—O1^xiii	99.53 (2)
O2^vi—O1—O2^vii	117.06 (2)	Co—O3—O1ⁱⁱⁱ	41.755 (11)
O3^vii—O1—O2^vii	59.087 (18)	Co^iv—O3—O1ⁱⁱⁱ	121.57 (2)
O2^viii—O1—O2^vii	45.008 (18)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	48.540 (14)
O3^ix—O1—O2^vii	101.679 (19)	O2^xiii—O3—O1ⁱⁱⁱ	146.231 (15)
O2^x—O1—O2^vii	81.162 (15)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	86.886 (18)
S—O1—O3^xi	103.82 (3)	O1^vii—O3—O1ⁱⁱⁱ	80.404 (16)
Co^vi—O1—O3^xi	97.068 (18)	O2^xiv—O3—O1ⁱⁱⁱ	127.381 (15)
O2—O1—O3^xi	118.86 (2)	O2ⁱ—O3—O1ⁱⁱⁱ	60.415 (15)
O1^iv—O1—O3^xi	68.811 (10)	O2^iv—O3—O1ⁱⁱⁱ	99.53 (2)
O2^iv—O1—O3^xi	118.26 (2)	O2—O3—O1ⁱⁱⁱ	53.982 (14)
O2^vi—O1—O3^xi	51.511 (15)	O1^xiii—O3—O1ⁱⁱⁱ	153.41 (3)
O3^vii—O1—O3^xi	82.249 (17)	Co—O3—H	105.2 (10)
O2^viii—O1—O3^xi	138.021 (18)	Co^iv—O3—H	108.6 (10)
O3^ix—O1—O3^xi	106.914 (18)	O2ⁱⁱⁱ—O3—H	18.3 (11)
O2^x—O1—O3^xi	52.448 (13)	O2^xiii—O3—H	120.5 (11)
O2^vii—O1—O3^xi	132.722 (17)	O1ⁱⁱ—O3—H	145.3 (10)
S—O2—Co	131.98 (3)	O1^vii—O3—H	75.8 (10)
S—O2—O1	35.360 (16)	O2^xiv—O3—H	73.5 (10)
Co—O2—O1	161.18 (3)	O2ⁱ—O3—H	89.3 (10)
S—O2—O1^iv	34.745 (16)	O2^iv—O3—H	136.2 (10)
Co—O2—O1^iv	118.76 (2)	O2—O3—H	112.5 (11)
O1—O2—O1^iv	59.83 (3)	O1^xiii—O3—H	132.9 (10)
S—O2—O2^iv	35.352 (19)	O1ⁱⁱⁱ—O3—H	66.2 (11)
Co—O2—O2^iv	102.103 (17)	Co—O3—H^iv	108.6 (10)
O1—O2—O2^iv	60.190 (19)	Co^iv—O3—H^iv	105.2 (10)
O1^iv—O2—O2^iv	59.435 (18)	O2ⁱⁱⁱ—O3—H^iv	120.5 (11)
S—O2—O3^ix	108.25 (3)	O2^xiii—O3—H^iv	18.3 (11)
Co—O2—O3^ix	119.50 (2)	O1ⁱⁱ—O3—H^iv	75.8 (10)
O1—O2—O3^ix	74.01 (2)	O1^vii—O3—H^iv	145.3 (10)
O1^iv—O2—O3^ix	113.70 (3)	O2^xiv—O3—H^iv	89.3 (10)
O2^iv—O2—O3^ix	130.16 (3)	O2ⁱ—O3—H^iv	73.5 (10)
S—O2—O1ⁱⁱⁱ	160.23 (3)	O2^iv—O3—H^iv	112.5 (11)
Co—O2—O1ⁱⁱⁱ	47.272 (15)	O2—O3—H^iv	136.2 (10)
O1—O2—O1ⁱⁱⁱ	137.19 (2)	O1^xiii—O3—H^iv	66.2 (11)
O1^iv—O2—O1ⁱⁱⁱ	162.50 (3)	O1ⁱⁱⁱ—O3—H^iv	132.9 (10)
O2^iv—O2—O1ⁱⁱⁱ	128.159 (16)	H—O3—H^iv	106 (2)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x, y, −z+1/2; (v) x, −y+1, z−1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) x, y−1, z; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.839 (15)	1.923 (15)	2.7015 (6)	153.9 (15)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(CoSO4H2O_N2_153K) top

Crystal data top

CoH₂O₅S	V = 353.42 (9) Å³
M_r = 173.01	Z = 4
Monoclinic, C2/c	F(000) = 340
a = 6.9354 (10) Å	D_x = 3.251 Mg m⁻³
b = 7.6179 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.6043 (10) Å	µ = 5.33 mm⁻¹
β = 118.397 (10)°	T = 153 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.020
T_min = 0.577, T_max = 0.748	θ_max = 40.0°, θ_min = 4.2°
11432 measured reflections	h = −12→12
1098 independent reflections	k = −13→13
1089 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.012	w = 1/[σ²(F_o²) + (0.011P)² + 0.320P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.030	(Δ/σ)_max < 0.001
S = 1.14	Δρ_max = 0.52 e Å⁻³
1098 reflections	Δρ_min = −0.48 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0182 (8)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co	0.000000	0.500000	0.000000	0.00391 (3)
S	0.000000	0.15498 (3)	0.250000	0.00364 (4)
O1	0.17219 (7)	0.04444 (7)	0.40161 (7)	0.00767 (7)
O2	0.09929 (7)	0.26795 (6)	0.15505 (7)	0.00672 (7)
O3	0.000000	0.63789 (9)	0.250000	0.00618 (9)
H	0.110 (2)	0.705 (2)	0.293 (2)	0.019 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co	0.00381 (5)	0.00393 (5)	0.00408 (5)	−0.00008 (3)	0.00195 (3)	0.00027 (3)
S	0.00310 (7)	0.00347 (7)	0.00437 (7)	0.000	0.00180 (5)	0.000
O1	0.00509 (15)	0.00865 (17)	0.00855 (16)	0.00232 (13)	0.00265 (13)	0.00426 (13)
O2	0.00699 (16)	0.00600 (16)	0.00904 (16)	0.00071 (12)	0.00532 (13)	0.00279 (12)
O3	0.0061 (2)	0.0065 (2)	0.0063 (2)	0.000	0.00327 (17)	0.000

Geometric parameters (Å, º) top

Co—O2ⁱ	2.0535 (5)	O1—O1^iv	2.4048 (10)
Co—O2	2.0535 (5)	O1—O2^iv	2.4204 (7)
Co—O1ⁱⁱ	2.0555 (6)	O1—O2^vi	2.7899 (7)
Co—O1ⁱⁱⁱ	2.0555 (6)	O1—O3^vii	2.8962 (7)
Co—O3ⁱ	2.1720 (4)	O1—O2^viii	3.0168 (8)
Co—O3	2.1720 (4)	O1—O3^ix	3.0818 (6)
Co—O2ⁱⁱⁱ	3.4405 (6)	O1—O2^x	3.2496 (7)
Co—O2ⁱⁱ	3.4405 (6)	O1—O2^vii	3.2921 (8)
Co—O2^iv	3.4925 (6)	O1—O3^xi	3.3223 (9)
Co—O2^v	3.4925 (6)	O2—O2^iv	2.4235 (9)
S—O1	1.4679 (5)	O2—O3^ix	2.7052 (6)
S—O1^iv	1.4679 (5)	O2—O3ⁱ	2.9084 (6)
S—O2	1.4863 (5)	O2—O3	3.0677 (8)
S—O2^iv	1.4863 (5)	O3—H	0.846 (15)
O1—O2	2.4017 (7)	O3—H^iv	0.846 (15)

O2ⁱ—Co—O2	180.00 (3)	O3^ix—O2—O1ⁱⁱⁱ	74.38 (2)
O2ⁱ—Co—O1ⁱⁱ	85.52 (2)	S—O2—O3ⁱ	136.57 (3)
O2—Co—O1ⁱⁱ	94.47 (2)	Co—O2—O3ⁱ	48.223 (16)
O2ⁱ—Co—O1ⁱⁱⁱ	94.48 (2)	O1—O2—O3ⁱ	149.04 (3)
O2—Co—O1ⁱⁱⁱ	85.53 (2)	O1^iv—O2—O3ⁱ	102.28 (2)
O1ⁱⁱ—Co—O1ⁱⁱⁱ	180.00 (3)	O2^iv—O2—O3ⁱ	135.69 (3)
O2ⁱ—Co—O3ⁱ	93.06 (2)	O3^ix—O2—O3ⁱ	93.942 (19)
O2—Co—O3ⁱ	86.94 (2)	O1ⁱⁱⁱ—O2—O3ⁱ	61.053 (17)
O1ⁱⁱ—Co—O3ⁱ	93.563 (16)	S—O2—O1ⁱⁱ	92.50 (2)
O1ⁱⁱⁱ—Co—O3ⁱ	86.437 (16)	Co—O2—O1ⁱⁱ	42.788 (13)
O2ⁱ—Co—O3	86.94 (2)	O1—O2—O1ⁱⁱ	127.79 (3)
O2—Co—O3	93.06 (2)	O1^iv—O2—O1ⁱⁱ	77.01 (2)
O1ⁱⁱ—Co—O3	86.437 (16)	O2^iv—O2—O1ⁱⁱ	73.57 (2)
O1ⁱⁱⁱ—Co—O3	93.563 (16)	O3^ix—O2—O1ⁱⁱ	156.34 (2)
O3ⁱ—Co—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.06 (2)
O2ⁱ—Co—O2ⁱⁱⁱ	81.706 (13)	O3ⁱ—O2—O1ⁱⁱ	62.650 (17)
O2—Co—O2ⁱⁱⁱ	98.294 (13)	S—O2—O3	102.12 (2)
O1ⁱⁱ—Co—O2ⁱⁱⁱ	136.701 (16)	Co—O2—O3	44.993 (13)
O1ⁱⁱⁱ—Co—O2ⁱⁱⁱ	43.299 (16)	O1—O2—O3	117.07 (2)
O3ⁱ—Co—O2ⁱⁱⁱ	128.172 (13)	O1^iv—O2—O3	116.45 (2)
O3—Co—O2ⁱⁱⁱ	51.828 (13)	O2^iv—O2—O3	66.733 (10)
O2ⁱ—Co—O2ⁱⁱ	98.294 (14)	O3^ix—O2—O3	126.21 (2)
O2—Co—O2ⁱⁱ	81.705 (13)	O1ⁱⁱⁱ—O2—O3	63.279 (17)
O1ⁱⁱ—Co—O2ⁱⁱ	43.299 (16)	O3ⁱ—O2—O3	93.216 (16)
O1ⁱⁱⁱ—Co—O2ⁱⁱ	136.701 (16)	O1ⁱⁱ—O2—O3	56.841 (14)
O3ⁱ—Co—O2ⁱⁱ	51.828 (13)	S—O2—O1^xii	95.90 (3)
O3—Co—O2ⁱⁱ	128.172 (13)	Co—O2—O1^xii	113.21 (2)
O2ⁱⁱⁱ—Co—O2ⁱⁱ	180.0	O1—O2—O1^xii	84.804 (17)
O2ⁱ—Co—O2^iv	137.297 (17)	O1^iv—O2—O1^xii	72.93 (2)
O2—Co—O2^iv	42.702 (17)	O2^iv—O2—O1^xii	130.253 (15)
O1ⁱⁱ—Co—O2^iv	67.109 (18)	O3^ix—O2—O1^xii	57.331 (16)
O1ⁱⁱⁱ—Co—O2^iv	112.891 (18)	O1ⁱⁱⁱ—O2—O1^xii	101.61 (2)
O3ⁱ—Co—O2^iv	119.647 (19)	O3ⁱ—O2—O1^xii	65.024 (19)
O3—Co—O2^iv	60.353 (19)	O1ⁱⁱ—O2—O1^xii	110.52 (2)
O2ⁱⁱⁱ—Co—O2^iv	95.968 (16)	O3—O2—O1^xii	158.125 (19)
O2ⁱⁱ—Co—O2^iv	84.032 (16)	S—O2—O1^vii	82.10 (2)
O2ⁱ—Co—O2^v	42.703 (18)	Co—O2—O1^vii	94.64 (2)
O2—Co—O2^v	137.298 (17)	O1—O2—O1^vii	71.84 (2)
O1ⁱⁱ—Co—O2^v	112.891 (18)	O1^iv—O2—O1^vii	116.27 (2)
O1ⁱⁱⁱ—Co—O2^v	67.109 (18)	O2^iv—O2—O1^vii	61.51 (2)
O3ⁱ—Co—O2^v	60.353 (19)	O3^ix—O2—O1^vii	87.279 (19)
O3—Co—O2^v	119.647 (19)	O1ⁱⁱⁱ—O2—O1^vii	78.359 (16)
O2ⁱⁱⁱ—Co—O2^v	84.032 (16)	O3ⁱ—O2—O1^vii	137.19 (2)
O2ⁱⁱ—Co—O2^v	95.968 (16)	O1ⁱⁱ—O2—O1^vii	107.26 (2)
O2^iv—Co—O2^v	180.000 (13)	O3—O2—O1^vii	54.040 (12)
O1—S—O1^iv	109.99 (4)	O1^xii—O2—O1^vii	142.217 (18)
O1—S—O2	108.78 (3)	Co—O3—Co^iv	122.15 (3)
O1^iv—S—O2	110.03 (3)	Co—O3—O2^xiii	111.787 (14)
O1—S—O2^iv	110.03 (3)	Co^iv—O3—O2^xiii	89.032 (13)
O1^iv—S—O2^iv	108.78 (3)	Co—O3—O2ⁱⁱⁱ	89.032 (13)
O2—S—O2^iv	109.23 (4)	Co^iv—O3—O2ⁱⁱⁱ	111.787 (14)
S—O1—Co^vi	136.57 (3)	O2^xiii—O3—O2ⁱⁱⁱ	137.03 (3)
S—O1—O2	35.867 (17)	Co—O3—O1ⁱⁱ	45.102 (13)
Co^vi—O1—O2	100.76 (2)	Co^iv—O3—O1ⁱⁱ	104.00 (2)
S—O1—O1^iv	35.00 (2)	O2^xiii—O3—O1ⁱⁱ	70.829 (17)
Co^vi—O1—O1^iv	140.47 (3)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	132.819 (16)
O2—O1—O1^iv	60.47 (2)	Co—O3—O1^vii	104.00 (2)
S—O1—O2^iv	35.236 (17)	Co^iv—O3—O1^vii	45.102 (13)
Co^vi—O1—O2^iv	144.37 (3)	O2^xiii—O3—O1^vii	132.820 (16)
O2—O1—O2^iv	60.34 (2)	O2ⁱⁱⁱ—O3—O1^vii	70.829 (17)
O1^iv—O1—O2^iv	59.701 (19)	O1ⁱⁱ—O3—O1^vii	122.68 (3)
S—O1—O2^vi	128.43 (3)	Co—O3—O2^xiv	161.39 (2)
Co^vi—O1—O2^vi	47.208 (14)	Co^iv—O3—O2^xiv	44.835 (12)
O2—O1—O2^vi	109.80 (2)	O2^xiii—O3—O2^xiv	83.575 (17)
O1^iv—O1—O2^vi	103.30 (2)	O2ⁱⁱⁱ—O3—O2^xiv	86.058 (18)
O2^iv—O1—O2^vi	162.66 (3)	O1ⁱⁱ—O3—O2^xiv	140.764 (17)
S—O1—O3^vii	170.08 (3)	O1^vii—O3—O2^xiv	57.453 (16)
Co^vi—O1—O3^vii	48.461 (12)	Co—O3—O2ⁱ	44.835 (12)
O2—O1—O3^vii	146.76 (2)	Co^iv—O3—O2ⁱ	161.39 (2)
O1^iv—O1—O3^vii	150.078 (18)	O2^xiii—O3—O2ⁱ	86.058 (18)
O2^iv—O1—O3^vii	134.91 (2)	O2ⁱⁱⁱ—O3—O2ⁱ	83.575 (17)
O2^vi—O1—O3^vii	61.492 (18)	O1ⁱⁱ—O3—O2ⁱ	57.453 (16)
S—O1—O2^viii	114.51 (3)	O1^vii—O3—O2ⁱ	140.764 (17)
Co^vi—O1—O2^viii	42.736 (15)	O2^xiv—O3—O2ⁱ	151.45 (3)
O2—O1—O2^viii	86.62 (2)	Co—O3—O2^iv	81.67 (2)
O1^iv—O1—O2^viii	146.96 (2)	Co^iv—O3—O2^iv	41.948 (14)
O2^iv—O1—O2^viii	102.99 (2)	O2^xiii—O3—O2^iv	94.714 (14)
O2^vi—O1—O2^viii	89.94 (2)	O2ⁱⁱⁱ—O3—O2^iv	126.21 (2)
O3^vii—O1—O2^viii	62.46 (2)	O1ⁱⁱ—O3—O2^iv	66.938 (19)
S—O1—O3^ix	92.47 (2)	O1^vii—O3—O2^iv	60.694 (18)
Co^vi—O1—O3^ix	44.702 (13)	O2^xiv—O3—O2^iv	86.783 (16)
O2—O1—O3^ix	57.527 (18)	O2ⁱ—O3—O2^iv	120.61 (2)
O1^iv—O1—O3^ix	102.38 (3)	Co—O3—O2	41.948 (14)
O2^iv—O1—O3^ix	114.88 (2)	Co^iv—O3—O2	81.67 (2)
O2^vi—O1—O3^ix	62.761 (19)	O2^xiii—O3—O2	126.21 (2)
O3^vii—O1—O3^ix	93.162 (19)	O2ⁱⁱⁱ—O3—O2	94.714 (14)
O2^viii—O1—O3^ix	56.953 (16)	O1ⁱⁱ—O3—O2	60.694 (18)
S—O1—O2^x	126.01 (3)	O1^vii—O3—O2	66.938 (19)
Co^vi—O1—O2^x	96.928 (19)	O2^xiv—O3—O2	120.61 (2)
O2—O1—O2^x	161.40 (3)	O2ⁱ—O3—O2	86.784 (16)
O1^iv—O1—O2^x	101.82 (2)	O2^iv—O3—O2	46.53 (2)
O2^iv—O1—O2^x	107.07 (2)	Co—O3—O1^xiii	121.52 (2)
O2^vi—O1—O2^x	78.39 (2)	Co^iv—O3—O1^xiii	41.735 (11)
O3^vii—O1—O2^x	51.839 (16)	O2^xiii—O3—O1^xiii	48.505 (15)
O2^viii—O1—O2^x	110.52 (2)	O2ⁱⁱⁱ—O3—O1^xiii	146.280 (16)
O3^ix—O1—O2^x	137.86 (2)	O1ⁱⁱ—O3—O1^xiii	80.421 (17)
S—O1—O2^vii	111.77 (3)	O1^vii—O3—O1^xiii	86.837 (19)
Co^vi—O1—O2^vii	77.777 (19)	O2^xiv—O3—O1^xiii	60.397 (15)
O2—O1—O2^vii	108.17 (2)	O2ⁱ—O3—O1^xiii	127.440 (16)
O1^iv—O1—O2^vii	139.18 (2)	O2^iv—O3—O1^xiii	53.959 (14)
O2^iv—O1—O2^vii	80.317 (19)	O2—O3—O1^xiii	99.43 (2)
O2^vi—O1—O2^vii	116.98 (2)	Co—O3—O1ⁱⁱⁱ	41.735 (11)
O3^vii—O1—O2^vii	59.021 (18)	Co^iv—O3—O1ⁱⁱⁱ	121.52 (2)
O2^viii—O1—O2^vii	44.918 (18)	O2^xiii—O3—O1ⁱⁱⁱ	146.280 (16)
O3^ix—O1—O2^vii	101.612 (19)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	48.505 (15)
O2^x—O1—O2^vii	81.112 (15)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	86.837 (19)
S—O1—O3^xi	103.78 (3)	O1^vii—O3—O1ⁱⁱⁱ	80.421 (17)
Co^vi—O1—O3^xi	97.215 (19)	O2^xiv—O3—O1ⁱⁱⁱ	127.440 (16)
O2—O1—O3^xi	118.85 (2)	O2ⁱ—O3—O1ⁱⁱⁱ	60.397 (15)
O1^iv—O1—O3^xi	68.781 (10)	O2^iv—O3—O1ⁱⁱⁱ	99.44 (2)
O2^iv—O1—O3^xi	118.24 (2)	O2—O3—O1ⁱⁱⁱ	53.959 (14)
O2^vi—O1—O3^xi	51.645 (16)	O1^xiii—O3—O1ⁱⁱⁱ	153.29 (3)
O3^vii—O1—O3^xi	82.333 (17)	Co—O3—H	104.7 (10)
O2^viii—O1—O3^xi	138.160 (18)	Co^iv—O3—H	109.4 (10)
O3^ix—O1—O3^xi	107.032 (19)	O2^xiii—O3—H	120.5 (10)
O2^x—O1—O3^xi	52.518 (14)	O2ⁱⁱⁱ—O3—H	18.2 (10)
O2^vii—O1—O3^xi	132.734 (17)	O1ⁱⁱ—O3—H	144.6 (10)
S—O2—Co	132.15 (3)	O1^vii—O3—H	76.4 (10)
S—O2—O1	35.357 (17)	O2^xiv—O3—H	74.2 (10)
Co—O2—O1	161.28 (3)	O2ⁱ—O3—H	88.5 (10)
S—O2—O1^iv	34.738 (17)	O2^iv—O3—H	136.7 (10)
Co—O2—O1^iv	118.90 (3)	O2—O3—H	112.5 (10)
O1—O2—O1^iv	59.83 (3)	O1^xiii—O3—H	133.5 (10)
S—O2—O2^iv	35.38 (2)	O1ⁱⁱⁱ—O3—H	65.8 (10)
Co—O2—O2^iv	102.222 (18)	Co—O3—H^iv	109.3 (10)
O1—O2—O2^iv	60.211 (19)	Co^iv—O3—H^iv	104.7 (10)
O1^iv—O2—O2^iv	59.449 (19)	O2^xiii—O3—H^iv	18.2 (10)
S—O2—O3^ix	108.23 (3)	O2ⁱⁱⁱ—O3—H^iv	120.5 (10)
Co—O2—O3^ix	119.34 (2)	O1ⁱⁱ—O3—H^iv	76.4 (10)
O1—O2—O3^ix	73.97 (2)	O1^vii—O3—H^iv	144.6 (10)
O1^iv—O2—O3^ix	113.79 (3)	O2^xiv—O3—H^iv	88.5 (10)
O2^iv—O2—O3^ix	130.07 (3)	O2ⁱ—O3—H^iv	74.2 (10)
S—O2—O1ⁱⁱⁱ	160.16 (3)	O2^iv—O3—H^iv	112.5 (10)
Co—O2—O1ⁱⁱⁱ	47.267 (16)	O2—O3—H^iv	136.7 (10)
O1—O2—O1ⁱⁱⁱ	137.02 (2)	O1^xiii—O3—H^iv	65.8 (10)
O1^iv—O2—O1ⁱⁱⁱ	162.66 (3)	O1ⁱⁱⁱ—O3—H^iv	133.5 (10)
O2^iv—O2—O1ⁱⁱⁱ	128.137 (16)	H—O3—H^iv	106 (2)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x, y, −z+1/2; (v) x, −y+1, z−1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) x, y−1, z; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.846 (15)	1.920 (15)	2.7051 (6)	154.0 (15)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(CoSO4H2O_N2_193K) top

Crystal data top

CoH₂O₅S	V = 353.72 (9) Å³
M_r = 173.01	Z = 4
Monoclinic, C2/c	F(000) = 340
a = 6.9432 (10) Å	D_x = 3.249 Mg m⁻³
b = 7.6126 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.6107 (10) Å	µ = 5.32 mm⁻¹
β = 118.441 (10)°	T = 193 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.020
T_min = 0.579, T_max = 0.748	θ_max = 40.0°, θ_min = 4.2°
11405 measured reflections	h = −12→12
1098 independent reflections	k = −13→13
1089 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.012	w = 1/[σ²(F_o²) + (0.012P)² + 0.280P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.030	(Δ/σ)_max < 0.001
S = 1.14	Δρ_max = 0.48 e Å⁻³
1098 reflections	Δρ_min = −0.46 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0206 (9)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co	0.000000	0.500000	0.000000	0.00474 (3)
S	0.000000	0.15468 (2)	0.250000	0.00432 (4)
O1	0.17231 (7)	0.04404 (7)	0.40123 (7)	0.00913 (7)
O2	0.09866 (7)	0.26764 (6)	0.15475 (7)	0.00793 (7)
O3	0.000000	0.63806 (9)	0.250000	0.00719 (9)
H	0.110 (2)	0.705 (2)	0.294 (2)	0.020 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co	0.00454 (5)	0.00472 (5)	0.00503 (5)	−0.00008 (3)	0.00235 (3)	0.00034 (3)
S	0.00356 (7)	0.00404 (7)	0.00533 (7)	0.000	0.00210 (5)	0.000
O1	0.00576 (15)	0.01036 (18)	0.01044 (17)	0.00267 (13)	0.00319 (13)	0.00513 (14)
O2	0.00812 (16)	0.00695 (16)	0.01093 (16)	0.00101 (12)	0.00634 (13)	0.00341 (13)
O3	0.0071 (2)	0.0076 (2)	0.0072 (2)	0.000	0.00371 (17)	0.000

Geometric parameters (Å, º) top

Co—O2ⁱ	2.0535 (5)	O1—O1^iv	2.4037 (10)
Co—O2	2.0535 (5)	O1—O2^iv	2.4197 (7)
Co—O1ⁱⁱ	2.0555 (6)	O1—O2^vi	2.7898 (7)
Co—O1ⁱⁱⁱ	2.0555 (6)	O1—O3^vii	2.8968 (7)
Co—O3ⁱ	2.1736 (4)	O1—O2^viii	3.0167 (8)
Co—O3	2.1736 (4)	O1—O3^ix	3.0835 (6)
Co—O2ⁱⁱⁱ	3.4418 (6)	O1—O2^x	3.2486 (7)
Co—O2ⁱⁱ	3.4418 (6)	O1—O2^vii	3.2993 (8)
Co—O2^iv	3.4953 (6)	O1—O3^xi	3.3161 (9)
Co—O2^v	3.4953 (6)	O2—O2^iv	2.4231 (9)
S—O1^iv	1.4676 (5)	O2—O3^ix	2.7091 (6)
S—O1	1.4676 (5)	O2—O3ⁱ	2.9093 (6)
S—O2	1.4857 (5)	O2—O3	3.0691 (8)
S—O2^iv	1.4857 (5)	O3—H	0.847 (15)
O1—O2	2.4008 (7)	O3—H^iv	0.847 (15)

O2ⁱ—Co—O2	180.0	O3^ix—O2—O1ⁱⁱⁱ	74.16 (2)
O2ⁱ—Co—O1ⁱⁱ	85.52 (2)	S—O2—O3ⁱ	136.78 (3)
O2—Co—O1ⁱⁱ	94.48 (2)	Co—O2—O3ⁱ	48.251 (16)
O2ⁱ—Co—O1ⁱⁱⁱ	94.48 (2)	O1—O2—O3ⁱ	149.03 (3)
O2—Co—O1ⁱⁱⁱ	85.52 (2)	O1^iv—O2—O3ⁱ	102.47 (2)
O1ⁱⁱ—Co—O1ⁱⁱⁱ	180.0	O2^iv—O2—O3ⁱ	135.93 (3)
O2ⁱ—Co—O3ⁱ	93.07 (2)	O3^ix—O2—O3ⁱ	93.824 (18)
O2—Co—O3ⁱ	86.93 (2)	O1ⁱⁱⁱ—O2—O3ⁱ	61.059 (17)
O1ⁱⁱ—Co—O3ⁱ	93.581 (16)	S—O2—O1ⁱⁱ	92.70 (2)
O1ⁱⁱⁱ—Co—O3ⁱ	86.419 (16)	Co—O2—O1ⁱⁱ	42.787 (13)
O2ⁱ—Co—O3	86.93 (2)	O1—O2—O1ⁱⁱ	128.00 (3)
O2—Co—O3	93.07 (2)	O1^iv—O2—O1ⁱⁱ	77.16 (2)
O1ⁱⁱ—Co—O3	86.419 (16)	O2^iv—O2—O1ⁱⁱ	73.77 (2)
O1ⁱⁱⁱ—Co—O3	93.581 (16)	O3^ix—O2—O1ⁱⁱ	156.23 (2)
O3ⁱ—Co—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.06 (2)
O2ⁱ—Co—O2ⁱⁱⁱ	81.697 (13)	O3ⁱ—O2—O1ⁱⁱ	62.678 (17)
O2—Co—O2ⁱⁱⁱ	98.303 (14)	S—O2—O3	102.11 (2)
O1ⁱⁱ—Co—O2ⁱⁱⁱ	136.757 (16)	Co—O2—O3	45.009 (12)
O1ⁱⁱⁱ—Co—O2ⁱⁱⁱ	43.243 (16)	O1—O2—O3	117.08 (2)
O3ⁱ—Co—O2ⁱⁱⁱ	128.095 (13)	O1^iv—O2—O3	116.46 (2)
O3—Co—O2ⁱⁱⁱ	51.905 (13)	O2^iv—O2—O3	66.749 (10)
O2ⁱ—Co—O2ⁱⁱ	98.303 (14)	O3^ix—O2—O3	126.03 (2)
O2—Co—O2ⁱⁱ	81.697 (14)	O1ⁱⁱⁱ—O2—O3	63.299 (17)
O1ⁱⁱ—Co—O2ⁱⁱ	43.243 (16)	O3ⁱ—O2—O3	93.260 (16)
O1ⁱⁱⁱ—Co—O2ⁱⁱ	136.757 (16)	O1ⁱⁱ—O2—O3	56.841 (13)
O3ⁱ—Co—O2ⁱⁱ	51.905 (13)	S—O2—O1^xii	96.12 (3)
O3—Co—O2ⁱⁱ	128.095 (13)	Co—O2—O1^xii	113.10 (2)
O2ⁱⁱⁱ—Co—O2ⁱⁱ	180.0	O1—O2—O1^xii	84.897 (17)
O2ⁱ—Co—O2^iv	137.375 (17)	O1^iv—O2—O1^xii	73.19 (2)
O2—Co—O2^iv	42.624 (17)	O2^iv—O2—O1^xii	130.479 (15)
O1ⁱⁱ—Co—O2^iv	67.249 (19)	O3^ix—O2—O1^xii	57.330 (17)
O1ⁱⁱⁱ—Co—O2^iv	112.751 (19)	O1ⁱⁱⁱ—O2—O1^xii	101.41 (2)
O3ⁱ—Co—O2^iv	119.674 (19)	O3ⁱ—O2—O1^xii	64.891 (19)
O3—Co—O2^iv	60.326 (19)	O1ⁱⁱ—O2—O1^xii	110.57 (2)
O2ⁱⁱⁱ—Co—O2^iv	95.908 (15)	O3—O2—O1^xii	158.019 (19)
O2ⁱⁱ—Co—O2^iv	84.092 (15)	S—O2—O1^vii	82.01 (2)
O2ⁱ—Co—O2^v	42.625 (17)	Co—O2—O1^vii	94.56 (2)
O2—Co—O2^v	137.376 (17)	O1—O2—O1^vii	71.84 (2)
O1ⁱⁱ—Co—O2^v	112.751 (19)	O1^iv—O2—O1^vii	116.17 (2)
O1ⁱⁱⁱ—Co—O2^v	67.249 (19)	O2^iv—O2—O1^vii	61.39 (2)
O3ⁱ—Co—O2^v	60.326 (19)	O3^ix—O2—O1^vii	87.223 (19)
O3—Co—O2^v	119.674 (19)	O1ⁱⁱⁱ—O2—O1^vii	78.285 (17)
O2ⁱⁱⁱ—Co—O2^v	84.092 (15)	O3ⁱ—O2—O1^vii	137.13 (2)
O2ⁱⁱ—Co—O2^v	95.908 (15)	O1ⁱⁱ—O2—O1^vii	107.22 (2)
O2^iv—Co—O2^v	180.000 (13)	O3—O2—O1^vii	53.968 (13)
O1^iv—S—O1	109.95 (4)	O1^xii—O2—O1^vii	142.212 (18)
O1^iv—S—O2	110.04 (3)	Co—O3—Co^iv	122.17 (3)
O1—S—O2	108.77 (3)	Co—O3—O2ⁱⁱⁱ	88.939 (13)
O1^iv—S—O2^iv	108.77 (3)	Co^iv—O3—O2ⁱⁱⁱ	111.754 (14)
O1—S—O2^iv	110.04 (3)	Co—O3—O2^xiii	111.754 (14)
O2—S—O2^iv	109.27 (4)	Co^iv—O3—O2^xiii	88.940 (13)
S—O1—Co^vi	136.66 (3)	O2ⁱⁱⁱ—O3—O2^xiii	137.29 (3)
S—O1—O2	35.867 (17)	Co—O3—O1ⁱⁱ	45.087 (14)
Co^vi—O1—O2	100.85 (2)	Co^iv—O3—O1ⁱⁱ	104.08 (2)
S—O1—O1^iv	35.02 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	132.714 (16)
Co^vi—O1—O1^iv	140.70 (3)	O2^xiii—O3—O1ⁱⁱ	70.740 (18)
O2—O1—O1^iv	60.48 (2)	Co—O3—O1^vii	104.08 (2)
S—O1—O2^iv	35.227 (17)	Co^iv—O3—O1^vii	45.087 (13)
Co^vi—O1—O2^iv	144.25 (3)	O2ⁱⁱⁱ—O3—O1^vii	70.740 (18)
O2—O1—O2^iv	60.35 (2)	O2^xiii—O3—O1^vii	132.715 (16)
O1^iv—O1—O2^iv	59.701 (19)	O1ⁱⁱ—O3—O1^vii	122.82 (3)
S—O1—O2^vi	128.62 (3)	Co—O3—O2^xiv	161.44 (2)
Co^vi—O1—O2^vi	47.208 (14)	Co^iv—O3—O2^xiv	44.816 (12)
O2—O1—O2^vi	109.89 (2)	O2ⁱⁱⁱ—O3—O2^xiv	86.176 (18)
O1^iv—O1—O2^vi	103.51 (2)	O2^xiii—O3—O2^xiv	83.511 (16)
O2^iv—O1—O2^vi	162.87 (3)	O1ⁱⁱ—O3—O2^xiv	140.754 (17)
S—O1—O3^vii	169.87 (3)	O1^vii—O3—O2^xiv	57.435 (17)
Co^vi—O1—O3^vii	48.494 (12)	Co—O3—O2ⁱ	44.816 (12)
O2—O1—O3^vii	146.86 (2)	Co^iv—O3—O2ⁱ	161.44 (2)
O1^iv—O1—O3^vii	150.081 (18)	O2ⁱⁱⁱ—O3—O2ⁱ	83.511 (17)
O2^iv—O1—O3^vii	134.71 (2)	O2^xiii—O3—O2ⁱ	86.175 (18)
O2^vi—O1—O3^vii	61.506 (17)	O1ⁱⁱ—O3—O2ⁱ	57.435 (17)
S—O1—O2^viii	114.45 (3)	O1^vii—O3—O2ⁱ	140.754 (17)
Co^vi—O1—O2^viii	42.736 (15)	O2^xiv—O3—O2ⁱ	151.43 (3)
O2—O1—O2^viii	86.66 (2)	Co—O3—O2^iv	81.70 (2)
O1^iv—O1—O2^viii	146.99 (2)	Co^iv—O3—O2^iv	41.923 (14)
O2^iv—O1—O2^viii	102.84 (2)	O2ⁱⁱⁱ—O3—O2^iv	126.03 (2)
O2^vi—O1—O2^viii	89.94 (2)	O2^xiii—O3—O2^iv	94.641 (14)
O3^vii—O1—O2^viii	62.49 (2)	O1ⁱⁱ—O3—O2^iv	67.08 (2)
S—O1—O3^ix	92.57 (2)	O1^vii—O3—O2^iv	60.669 (18)
Co^vi—O1—O3^ix	44.713 (13)	O2^xiv—O3—O2^iv	86.739 (16)
O2—O1—O3^ix	57.605 (18)	O2ⁱ—O3—O2^iv	120.69 (2)
O1^iv—O1—O3^ix	102.56 (3)	Co—O3—O2	41.923 (14)
O2^iv—O1—O3^ix	114.90 (2)	Co^iv—O3—O2	81.70 (2)
O2^vi—O1—O3^ix	62.773 (19)	O2ⁱⁱⁱ—O3—O2	94.641 (14)
O3^vii—O1—O3^ix	93.207 (19)	O2^xiii—O3—O2	126.03 (2)
O2^viii—O1—O3^ix	56.955 (16)	O1ⁱⁱ—O3—O2	60.669 (18)
S—O1—O2^x	125.79 (3)	O1^vii—O3—O2	67.08 (2)
Co^vi—O1—O2^x	97.098 (19)	O2^xiv—O3—O2	120.69 (2)
O2—O1—O2^x	161.20 (3)	O2ⁱ—O3—O2	86.739 (16)
O1^iv—O1—O2^x	101.67 (2)	O2^iv—O3—O2	46.50 (2)
O2^iv—O1—O2^x	106.81 (2)	Co—O3—O1^xiii	121.47 (2)
O2^vi—O1—O2^x	78.59 (2)	Co^iv—O3—O1^xiii	41.706 (11)
O3^vii—O1—O2^x	51.930 (15)	O2ⁱⁱⁱ—O3—O1^xiii	146.347 (16)
O2^viii—O1—O2^x	110.57 (2)	O2^xiii—O3—O1^xiii	48.442 (14)
O3^ix—O1—O2^x	138.08 (2)	O1ⁱⁱ—O3—O1^xiii	80.433 (17)
S—O1—O2^vii	111.66 (3)	O1^vii—O3—O1^xiii	86.793 (19)
Co^vi—O1—O2^vii	77.683 (19)	O2^xiv—O3—O1^xiii	60.367 (16)
O2—O1—O2^vii	108.16 (2)	O2ⁱ—O3—O1^xiii	127.516 (15)
O1^iv—O1—O2^vii	139.05 (2)	O2^iv—O3—O1^xiii	53.928 (14)
O2^iv—O1—O2^vii	80.20 (2)	O2—O3—O1^xiii	99.34 (2)
O2^vi—O1—O2^vii	116.90 (2)	Co—O3—O1ⁱⁱⁱ	41.706 (11)
O3^vii—O1—O2^vii	58.956 (19)	Co^iv—O3—O1ⁱⁱⁱ	121.47 (2)
O2^viii—O1—O2^vii	44.842 (18)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	48.442 (15)
O3^ix—O1—O2^vii	101.542 (19)	O2^xiii—O3—O1ⁱⁱⁱ	146.346 (16)
O2^x—O1—O2^vii	81.050 (15)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	86.793 (19)
S—O1—O3^xi	103.77 (3)	O1^vii—O3—O1ⁱⁱⁱ	80.433 (17)
Co^vi—O1—O3^xi	97.381 (19)	O2^xiv—O3—O1ⁱⁱⁱ	127.516 (15)
O2—O1—O3^xi	118.83 (2)	O2ⁱ—O3—O1ⁱⁱⁱ	60.367 (15)
O1^iv—O1—O3^xi	68.751 (10)	O2^iv—O3—O1ⁱⁱⁱ	99.34 (2)
O2^iv—O1—O3^xi	118.21 (2)	O2—O3—O1ⁱⁱⁱ	53.928 (14)
O2^vi—O1—O3^xi	51.809 (16)	O1^xiii—O3—O1ⁱⁱⁱ	153.16 (3)
O3^vii—O1—O3^xi	82.423 (17)	Co—O3—H	105.2 (10)
O2^viii—O1—O3^xi	138.316 (19)	Co^iv—O3—H	108.8 (10)
O3^ix—O1—O3^xi	107.166 (19)	O2ⁱⁱⁱ—O3—H	18.7 (10)
O2^x—O1—O3^xi	52.599 (14)	O2^xiii—O3—H	120.4 (10)
O2^vii—O1—O3^xi	132.743 (17)	O1ⁱⁱ—O3—H	145.1 (10)
S—O2—Co	132.30 (3)	O1^vii—O3—H	76.1 (10)
S—O2—O1	35.366 (16)	O2^xiv—O3—H	73.6 (10)
Co—O2—O1	161.37 (3)	O2ⁱ—O3—H	89.0 (10)
S—O2—O1^iv	34.738 (17)	O2^iv—O3—H	136.4 (10)
Co—O2—O1^iv	119.07 (3)	O2—O3—H	112.9 (10)
O1—O2—O1^iv	59.82 (3)	O1^xiii—O3—H	132.9 (10)
S—O2—O2^iv	35.36 (2)	O1ⁱⁱⁱ—O3—H	66.4 (10)
Co—O2—O2^iv	102.353 (18)	Co—O3—H^iv	108.8 (10)
O1—O2—O2^iv	60.21 (2)	Co^iv—O3—H^iv	105.3 (10)
O1^iv—O2—O2^iv	59.440 (19)	O2ⁱⁱⁱ—O3—H^iv	120.4 (10)
S—O2—O3^ix	108.25 (3)	O2^xiii—O3—H^iv	18.7 (10)
Co—O2—O3^ix	119.13 (2)	O1ⁱⁱ—O3—H^iv	76.1 (10)
O1—O2—O3^ix	73.95 (2)	O1^vii—O3—H^iv	145.1 (10)
O1^iv—O2—O3^ix	113.92 (3)	O2^xiv—O3—H^iv	89.0 (10)
O2^iv—O2—O3^ix	129.98 (3)	O2ⁱ—O3—H^iv	73.6 (10)
S—O2—O1ⁱⁱⁱ	160.03 (3)	O2^iv—O3—H^iv	112.9 (10)
Co—O2—O1ⁱⁱⁱ	47.268 (16)	O2—O3—H^iv	136.4 (10)
O1—O2—O1ⁱⁱⁱ	136.83 (2)	O1^xiii—O3—H^iv	66.4 (10)
O1^iv—O2—O1ⁱⁱⁱ	162.87 (3)	O1ⁱⁱⁱ—O3—H^iv	132.9 (10)
O2^iv—O2—O1ⁱⁱⁱ	128.113 (17)	H—O3—H^iv	105 (2)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x, y, −z+1/2; (v) x, −y+1, z−1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) x, y−1, z; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.847 (15)	1.927 (15)	2.7091 (6)	153.2 (14)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(CoSO4H2O_N2_233K) top

Crystal data top

CoH₂O₅S	V = 354.02 (9) Å³
M_r = 173.01	Z = 4
Monoclinic, C2/c	F(000) = 340
a = 6.9526 (10) Å	D_x = 3.246 Mg m⁻³
b = 7.6051 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.6184 (10) Å	µ = 5.32 mm⁻¹
β = 118.497 (10)°	T = 233 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.020
T_min = 0.577, T_max = 0.748	θ_max = 40.0°, θ_min = 4.2°
11496 measured reflections	h = −12→12
1101 independent reflections	k = −13→13
1095 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.012	w = 1/[σ²(F_o²) + (0.013P)² + 0.280P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.032	(Δ/σ)_max = 0.001
S = 1.16	Δρ_max = 0.47 e Å⁻³
1101 reflections	Δρ_min = −0.41 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0223 (10)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co	0.000000	0.500000	0.000000	0.00568 (4)
S	0.000000	0.15433 (3)	0.250000	0.00510 (4)
O1	0.17242 (8)	0.04355 (7)	0.40080 (8)	0.01078 (8)
O2	0.09802 (8)	0.26722 (6)	0.15443 (7)	0.00931 (8)
O3	0.000000	0.63819 (9)	0.250000	0.00832 (10)
H	0.103 (2)	0.704 (2)	0.294 (2)	0.026 (4)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co	0.00537 (5)	0.00567 (5)	0.00604 (5)	−0.00009 (3)	0.00275 (4)	0.00038 (3)
S	0.00412 (7)	0.00475 (7)	0.00634 (7)	0.000	0.00242 (5)	0.000
O1	0.00670 (16)	0.01221 (19)	0.01247 (18)	0.00322 (14)	0.00380 (14)	0.00609 (15)
O2	0.00939 (17)	0.00810 (17)	0.01282 (18)	0.00123 (13)	0.00722 (15)	0.00394 (14)
O3	0.0083 (2)	0.0087 (2)	0.0083 (2)	0.000	0.00431 (19)	0.000

Geometric parameters (Å, º) top

Co—O2	2.0537 (5)	O1—O1^v	2.4023 (11)
Co—O2ⁱ	2.0537 (5)	O1—O2^v	2.4189 (7)
Co—O1ⁱⁱ	2.0556 (6)	O1—O2^vi	2.7895 (8)
Co—O1ⁱⁱⁱ	2.0556 (6)	O1—O3^vii	2.8971 (7)
Co—O3ⁱ	2.1753 (4)	O1—O2^viii	3.0174 (8)
Co—O3	2.1753 (4)	O1—O3^ix	3.0857 (6)
Co—O2ⁱⁱ	3.4425 (6)	O1—O2^x	3.2466 (8)
Co—O2ⁱⁱⁱ	3.4425 (6)	O1—O2^vii	3.3075 (9)
Co—O2^iv	3.4988 (6)	O1—O3^xi	3.3085 (9)
Co—O2^v	3.4988 (6)	O2—O2^v	2.4233 (10)
S—O1^v	1.4672 (5)	O2—O3^ix	2.7134 (7)
S—O1	1.4672 (5)	O2—O3ⁱ	2.9106 (6)
S—O2	1.4850 (5)	O2—O3	3.0704 (9)
S—O2^v	1.4850 (5)	O3—H	0.808 (15)
O1—O2	2.3995 (7)	O3—H^v	0.808 (15)

O2—Co—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	73.90 (2)
O2—Co—O1ⁱⁱ	94.49 (2)	S—O2—O3ⁱ	137.01 (3)
O2ⁱ—Co—O1ⁱⁱ	85.50 (2)	Co—O2—O3ⁱ	48.272 (17)
O2—Co—O1ⁱⁱⁱ	85.51 (2)	O1—O2—O3ⁱ	149.03 (3)
O2ⁱ—Co—O1ⁱⁱⁱ	94.50 (2)	O1^v—O2—O3ⁱ	102.69 (3)
O1ⁱⁱ—Co—O1ⁱⁱⁱ	180.0	O2^v—O2—O3ⁱ	136.17 (3)
O2—Co—O3ⁱ	86.93 (2)	O3^ix—O2—O3ⁱ	93.693 (19)
O2ⁱ—Co—O3ⁱ	93.07 (2)	O1ⁱⁱⁱ—O2—O3ⁱ	61.052 (19)
O1ⁱⁱ—Co—O3ⁱ	93.616 (17)	S—O2—O1ⁱⁱ	92.89 (3)
O1ⁱⁱⁱ—Co—O3ⁱ	86.384 (17)	Co—O2—O1ⁱⁱ	42.777 (14)
O2—Co—O3	93.07 (2)	O1—O2—O1ⁱⁱ	128.21 (3)
O2ⁱ—Co—O3	86.93 (2)	O1^v—O2—O1ⁱⁱ	77.33 (3)
O1ⁱⁱ—Co—O3	86.384 (17)	O2^v—O2—O1ⁱⁱ	73.97 (3)
O1ⁱⁱⁱ—Co—O3	93.616 (17)	O3^ix—O2—O1ⁱⁱ	156.09 (2)
O3ⁱ—Co—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.05 (2)
O2—Co—O2ⁱⁱ	81.701 (13)	O3ⁱ—O2—O1ⁱⁱ	62.705 (18)
O2ⁱ—Co—O2ⁱⁱ	98.299 (14)	S—O2—O3	102.08 (3)
O1ⁱⁱ—Co—O2ⁱⁱ	43.188 (17)	Co—O2—O3	45.029 (13)
O1ⁱⁱⁱ—Co—O2ⁱⁱ	136.812 (17)	O1—O2—O3	117.09 (2)
O3ⁱ—Co—O2ⁱⁱ	52.000 (13)	O1^v—O2—O3	116.45 (2)
O3—Co—O2ⁱⁱ	128.000 (13)	O2^v—O2—O3	66.759 (11)
O2—Co—O2ⁱⁱⁱ	98.299 (14)	O3^ix—O2—O3	125.83 (2)
O2ⁱ—Co—O2ⁱⁱⁱ	81.701 (14)	O1ⁱⁱⁱ—O2—O3	63.335 (18)
O1ⁱⁱ—Co—O2ⁱⁱⁱ	136.812 (17)	O3ⁱ—O2—O3	93.300 (17)
O1ⁱⁱⁱ—Co—O2ⁱⁱⁱ	43.188 (17)	O1ⁱⁱ—O2—O3	56.827 (14)
O3ⁱ—Co—O2ⁱⁱⁱ	127.999 (13)	S—O2—O1^xii	96.41 (3)
O3—Co—O2ⁱⁱⁱ	52.001 (13)	Co—O2—O1^xii	112.96 (2)
O2ⁱⁱ—Co—O2ⁱⁱⁱ	180.0	O1—O2—O1^xii	85.031 (18)
O2—Co—O2^iv	137.452 (18)	O1^v—O2—O1^xii	73.50 (2)
O2ⁱ—Co—O2^iv	42.550 (19)	O2^v—O2—O1^xii	130.742 (16)
O1ⁱⁱ—Co—O2^iv	112.60 (2)	O3^ix—O2—O1^xii	57.333 (17)
O1ⁱⁱⁱ—Co—O2^iv	67.40 (2)	O1ⁱⁱⁱ—O2—O1^xii	101.16 (2)
O3ⁱ—Co—O2^iv	60.28 (2)	O3ⁱ—O2—O1^xii	64.74 (2)
O3—Co—O2^iv	119.72 (2)	O1ⁱⁱ—O2—O1^xii	110.61 (2)
O2ⁱⁱ—Co—O2^iv	95.840 (16)	O3—O2—O1^xii	157.88 (2)
O2ⁱⁱⁱ—Co—O2^iv	84.159 (16)	S—O2—O1^vii	81.91 (2)
O2—Co—O2^v	42.548 (18)	Co—O2—O1^vii	94.47 (2)
O2ⁱ—Co—O2^v	137.450 (18)	O1—O2—O1^vii	71.85 (3)
O1ⁱⁱ—Co—O2^v	67.40 (2)	O1^v—O2—O1^vii	116.06 (3)
O1ⁱⁱⁱ—Co—O2^v	112.60 (2)	O2^v—O2—O1^vii	61.26 (2)
O3ⁱ—Co—O2^v	119.72 (2)	O3^ix—O2—O1^vii	87.17 (2)
O3—Co—O2^v	60.28 (2)	O1ⁱⁱⁱ—O2—O1^vii	78.204 (17)
O2ⁱⁱ—Co—O2^v	84.160 (16)	O3ⁱ—O2—O1^vii	137.04 (2)
O2ⁱⁱⁱ—Co—O2^v	95.841 (16)	O1ⁱⁱ—O2—O1^vii	107.16 (2)
O2^iv—Co—O2^v	180.0	O3—O2—O1^vii	53.877 (13)
O1^v—S—O1	109.91 (5)	O1^xii—O2—O1^vii	142.226 (19)
O1^v—S—O2	110.05 (3)	Co—O3—Co^v	122.22 (3)
O1—S—O2	108.74 (3)	Co—O3—O2^xiii	111.718 (15)
O1^v—S—O2^v	108.74 (3)	Co^v—O3—O2^xiii	88.820 (13)
O1—S—O2^v	110.04 (3)	Co—O3—O2ⁱⁱⁱ	88.819 (14)
O2—S—O2^v	109.36 (4)	Co^v—O3—O2ⁱⁱⁱ	111.719 (15)
S—O1—Co^vi	136.76 (3)	O2^xiii—O3—O2ⁱⁱⁱ	137.60 (4)
S—O1—O2	35.878 (18)	Co—O3—O1ⁱⁱ	45.081 (14)
Co^vi—O1—O2	100.92 (2)	Co^v—O3—O1ⁱⁱ	104.19 (3)
S—O1—O1^v	35.05 (2)	O2^xiii—O3—O1ⁱⁱ	70.629 (19)
Co^vi—O1—O1^v	140.97 (4)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	132.590 (17)
O2—O1—O1^v	60.50 (2)	Co—O3—O1^vii	104.19 (3)
S—O1—O2^v	35.220 (19)	Co^v—O3—O1^vii	45.081 (15)
Co^vi—O1—O2^v	144.12 (3)	O2^xiii—O3—O1^vii	132.591 (17)
O2—O1—O2^v	60.38 (3)	O2ⁱⁱⁱ—O3—O1^vii	70.629 (18)
O1^v—O1—O2^v	59.69 (2)	O1ⁱⁱ—O3—O1^vii	123.01 (4)
S—O1—O2^vi	128.83 (3)	Co—O3—O2^xiv	161.52 (3)
Co^vi—O1—O2^vi	47.218 (15)	Co^v—O3—O2^xiv	44.795 (12)
O2—O1—O2^vi	109.96 (2)	O2^xiii—O3—O2^xiv	83.435 (18)
O1^v—O1—O2^vi	103.74 (2)	O2ⁱⁱⁱ—O3—O2^xiv	86.31 (2)
O2^v—O1—O2^vi	163.09 (3)	O1ⁱⁱ—O3—O2^xiv	140.754 (18)
S—O1—O3^vii	169.63 (3)	O1^vii—O3—O2^xiv	57.410 (18)
Co^vi—O1—O3^vii	48.535 (13)	Co—O3—O2ⁱ	44.795 (12)
O2—O1—O3^vii	146.94 (3)	Co^v—O3—O2ⁱ	161.52 (3)
O1^v—O1—O3^vii	150.098 (19)	O2^xiii—O3—O2ⁱ	86.306 (19)
O2^v—O1—O3^vii	134.47 (3)	O2ⁱⁱⁱ—O3—O2ⁱ	83.434 (18)
O2^vi—O1—O3^vii	61.537 (18)	O1ⁱⁱ—O3—O2ⁱ	57.410 (18)
S—O1—O2^viii	114.38 (3)	O1^vii—O3—O2ⁱ	140.754 (18)
Co^vi—O1—O2^viii	42.727 (16)	O2^xiv—O3—O2ⁱ	151.38 (3)
O2—O1—O2^viii	86.70 (2)	Co—O3—O2	41.905 (15)
O1^v—O1—O2^viii	147.01 (2)	Co^v—O3—O2	81.74 (2)
O2^v—O1—O2^viii	102.67 (3)	O2^xiii—O3—O2	125.83 (2)
O2^vi—O1—O2^viii	89.95 (2)	O2ⁱⁱⁱ—O3—O2	94.543 (15)
O3^vii—O1—O2^viii	62.51 (2)	O1ⁱⁱ—O3—O2	60.66 (2)
S—O1—O3^ix	92.69 (3)	O1^vii—O3—O2	67.25 (2)
Co^vi—O1—O3^ix	44.713 (14)	O2^xiv—O3—O2	120.78 (2)
O2—O1—O3^ix	57.682 (19)	O2ⁱ—O3—O2	86.700 (17)
O1^v—O1—O3^ix	102.77 (3)	Co—O3—O2^v	81.74 (2)
O2^v—O1—O3^ix	114.95 (3)	Co^v—O3—O2^v	41.904 (15)
O2^vi—O1—O3^ix	62.78 (2)	O2^xiii—O3—O2^v	94.542 (15)
O3^vii—O1—O3^ix	93.25 (2)	O2ⁱⁱⁱ—O3—O2^v	125.83 (2)
O2^viii—O1—O3^ix	56.953 (17)	O1ⁱⁱ—O3—O2^v	67.25 (2)
S—O1—O2^x	125.55 (3)	O1^vii—O3—O2^v	60.66 (2)
Co^vi—O1—O2^x	97.30 (2)	O2^xiv—O3—O2^v	86.700 (17)
O2—O1—O2^x	161.00 (3)	O2ⁱ—O3—O2^v	120.78 (2)
O1^v—O1—O2^x	101.51 (2)	O2—O3—O2^v	46.48 (2)
O2^v—O1—O2^x	106.50 (2)	Co—O3—O1^xiii	121.44 (2)
O2^vi—O1—O2^x	78.84 (2)	Co^v—O3—O1^xiii	41.670 (12)
O3^vii—O1—O2^x	52.038 (16)	O2^xiii—O3—O1^xiii	48.360 (15)
O2^viii—O1—O2^x	110.62 (2)	O2ⁱⁱⁱ—O3—O1^xiii	146.425 (17)
O3^ix—O1—O2^x	138.32 (2)	O1ⁱⁱ—O3—O1^xiii	80.451 (18)
S—O1—O2^vii	111.53 (3)	O1^vii—O3—O1^xiii	86.75 (2)
Co^vi—O1—O2^vii	77.58 (2)	O2^xiv—O3—O1^xiii	60.342 (16)
O2—O1—O2^vii	108.15 (3)	O2ⁱ—O3—O1^xiii	127.599 (16)
O1^v—O1—O2^vii	138.89 (3)	O2—O3—O1^xiii	99.25 (2)
O2^v—O1—O2^vii	80.06 (2)	O2^v—O3—O1^xiii	53.888 (15)
O2^vi—O1—O2^vii	116.82 (2)	Co—O3—O1ⁱⁱⁱ	41.670 (12)
O3^vii—O1—O2^vii	58.88 (2)	Co^v—O3—O1ⁱⁱⁱ	121.44 (2)
O2^viii—O1—O2^vii	44.764 (19)	O2^xiii—O3—O1ⁱⁱⁱ	146.425 (17)
O3^ix—O1—O2^vii	101.47 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	48.360 (15)
O2^x—O1—O2^vii	80.970 (16)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	86.75 (2)
S—O1—O3^xi	103.76 (3)	O1^vii—O3—O1ⁱⁱⁱ	80.451 (18)
Co^vi—O1—O3^xi	97.58 (2)	O2^xiv—O3—O1ⁱⁱⁱ	127.599 (16)
O2—O1—O3^xi	118.80 (3)	O2ⁱ—O3—O1ⁱⁱⁱ	60.342 (17)
O1^v—O1—O3^xi	68.713 (11)	O2—O3—O1ⁱⁱⁱ	53.888 (15)
O2^v—O1—O3^xi	118.17 (2)	O2^v—O3—O1ⁱⁱⁱ	99.25 (2)
O2^vi—O1—O3^xi	51.994 (17)	O1^xiii—O3—O1ⁱⁱⁱ	153.02 (3)
O3^vii—O1—O3^xi	82.542 (18)	Co—O3—H	107.2 (11)
O2^viii—O1—O3^xi	138.50 (2)	Co^v—O3—H	107.8 (11)
O3^ix—O1—O3^xi	107.31 (2)	O2^xiii—O3—H	118.9 (11)
O2^x—O1—O3^xi	52.710 (14)	O2ⁱⁱⁱ—O3—H	20.9 (11)
O2^vii—O1—O3^xi	132.762 (18)	O1ⁱⁱ—O3—H	146.6 (11)
S—O2—Co	132.44 (3)	O1^vii—O3—H	76.1 (11)
S—O2—O1	35.383 (17)	O2^xiv—O3—H	72.0 (11)
Co—O2—O1	161.44 (3)	O2ⁱ—O3—H	90.1 (11)
S—O2—O1^v	34.736 (19)	O2—O3—H	114.7 (11)
Co—O2—O1^v	119.25 (3)	O2^v—O3—H	136.7 (11)
O1—O2—O1^v	59.81 (3)	O1^xiii—O3—H	131.1 (11)
S—O2—O2^v	35.32 (2)	O1ⁱⁱⁱ—O3—H	68.5 (11)
Co—O2—O2^v	102.487 (19)	Co—O3—H^v	107.8 (11)
O1—O2—O2^v	60.20 (2)	Co^v—O3—H^v	107.2 (11)
O1^v—O2—O2^v	59.41 (2)	O2^xiii—O3—H^v	20.9 (11)
S—O2—O3^ix	108.32 (3)	O2ⁱⁱⁱ—O3—H^v	118.9 (11)
Co—O2—O3^ix	118.90 (2)	O1ⁱⁱ—O3—H^v	76.1 (11)
O1—O2—O3^ix	73.96 (2)	O1^vii—O3—H^v	146.6 (11)
O1^v—O2—O3^ix	114.08 (3)	O2^xiv—O3—H^v	90.1 (11)
O2^v—O2—O3^ix	129.90 (3)	O2ⁱ—O3—H^v	72.0 (11)
S—O2—O1ⁱⁱⁱ	159.88 (3)	O2—O3—H^v	136.7 (11)
Co—O2—O1ⁱⁱⁱ	47.276 (17)	O2^v—O3—H^v	114.7 (11)
O1—O2—O1ⁱⁱⁱ	136.61 (2)	O1^xiii—O3—H^v	68.5 (11)
O1^v—O2—O1ⁱⁱⁱ	163.09 (3)	O1ⁱⁱⁱ—O3—H^v	131.1 (11)
O2^v—O2—O1ⁱⁱⁱ	128.095 (18)	H—O3—H^v	103 (2)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x, −y+1, z−1/2; (v) −x, y, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) x, y−1, z; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.808 (15)	1.979 (15)	2.7134 (7)	150.8 (16)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(CoSO4H2O_N2_273K) top

Crystal data top

CoH₂O₅S	V = 354.56 (9) Å³
M_r = 173.01	Z = 4
Monoclinic, C2/c	F(000) = 340
a = 6.9641 (10) Å	D_x = 3.241 Mg m⁻³
b = 7.599 (1) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.6275 (10) Å	µ = 5.31 mm⁻¹
β = 118.553 (10)°	T = 273 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.019
T_min = 0.577, T_max = 0.748	θ_max = 40.0°, θ_min = 4.2°
11509 measured reflections	h = −12→12
1103 independent reflections	k = −13→13
1095 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.012	w = 1/[σ²(F_o²) + (0.013P)² + 0.260P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.032	(Δ/σ)_max < 0.001
S = 1.16	Δρ_max = 0.47 e Å⁻³
1103 reflections	Δρ_min = −0.42 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0229 (10)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co	0.000000	0.500000	0.000000	0.00667 (4)
S	0.000000	0.15394 (3)	0.250000	0.00590 (4)
O1	0.17252 (8)	0.04305 (8)	0.40031 (8)	0.01245 (8)
O2	0.09729 (8)	0.26680 (7)	0.15409 (8)	0.01077 (8)
O3	0.000000	0.63844 (9)	0.250000	0.00956 (10)
H	0.102 (2)	0.703 (2)	0.294 (2)	0.028 (4)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co	0.00626 (5)	0.00668 (5)	0.00709 (5)	−0.00011 (3)	0.00322 (4)	0.00044 (3)
S	0.00478 (7)	0.00550 (7)	0.00729 (7)	0.000	0.00277 (5)	0.000
O1	0.00762 (16)	0.0141 (2)	0.01452 (19)	0.00368 (15)	0.00439 (15)	0.00713 (16)
O2	0.01087 (17)	0.00944 (17)	0.01480 (19)	0.00154 (14)	0.00840 (15)	0.00458 (14)
O3	0.0095 (2)	0.0102 (2)	0.0096 (2)	0.000	0.00499 (19)	0.000

Geometric parameters (Å, º) top

Co—O2	2.0541 (5)	O1—O1^v	2.4010 (11)
Co—O2ⁱ	2.0541 (5)	O1—O2^v	2.4183 (8)
Co—O1ⁱⁱ	2.0564 (6)	O1—O2^vi	2.7901 (8)
Co—O1ⁱⁱⁱ	2.0564 (6)	O1—O3^vii	2.8987 (7)
Co—O3	2.1778 (4)	O1—O2^viii	3.0186 (8)
Co—O3ⁱ	2.1778 (4)	O1—O3^ix	3.0888 (6)
Co—O2ⁱⁱ	3.4444 (6)	O1—O2^x	3.2457 (8)
Co—O2ⁱⁱⁱ	3.4444 (6)	O1—O3^xi	3.3007 (10)
Co—O2^iv	3.5028 (6)	O1—O2^vii	3.3168 (9)
Co—O2^v	3.5028 (6)	O2—O2^v	2.4232 (10)
S—O1	1.4667 (5)	O2—O3^ix	2.7186 (7)
S—O1^v	1.4667 (5)	O2—O3ⁱ	2.9123 (7)
S—O2	1.4845 (5)	O2—O3	3.0730 (9)
S—O2^v	1.4845 (5)	O3—H	0.797 (15)
O1—O2	2.3983 (7)	O3—H^v	0.797 (15)

O2—Co—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	73.61 (2)
O2—Co—O1ⁱⁱ	94.51 (2)	S—O2—O3ⁱ	137.25 (3)
O2ⁱ—Co—O1ⁱⁱ	85.49 (2)	Co—O2—O3ⁱ	48.308 (17)
O2—Co—O1ⁱⁱⁱ	85.49 (2)	O1—O2—O3ⁱ	149.01 (3)
O2ⁱ—Co—O1ⁱⁱⁱ	94.51 (2)	O1^v—O2—O3ⁱ	102.92 (3)
O1ⁱⁱ—Co—O1ⁱⁱⁱ	180.00 (3)	O2^v—O2—O3ⁱ	136.44 (3)
O2—Co—O3	93.08 (2)	O3^ix—O2—O3ⁱ	93.540 (19)
O2ⁱ—Co—O3	86.92 (2)	O1ⁱⁱⁱ—O2—O3ⁱ	61.061 (19)
O1ⁱⁱ—Co—O3	86.356 (18)	S—O2—O1ⁱⁱ	93.12 (3)
O1ⁱⁱⁱ—Co—O3	93.644 (18)	Co—O2—O1ⁱⁱ	42.777 (14)
O2—Co—O3ⁱ	86.92 (2)	O1—O2—O1ⁱⁱ	128.45 (3)
O2ⁱ—Co—O3ⁱ	93.08 (2)	O1^v—O2—O1ⁱⁱ	77.50 (3)
O1ⁱⁱ—Co—O3ⁱ	93.644 (17)	O2^v—O2—O1ⁱⁱ	74.20 (3)
O1ⁱⁱⁱ—Co—O3ⁱ	86.356 (17)	O3^ix—O2—O1ⁱⁱ	155.93 (2)
O3—Co—O3ⁱ	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.06 (2)
O2—Co—O2ⁱⁱ	81.699 (13)	O3ⁱ—O2—O1ⁱⁱ	62.743 (18)
O2ⁱ—Co—O2ⁱⁱ	98.301 (14)	S—O2—O3	102.07 (3)
O1ⁱⁱ—Co—O2ⁱⁱ	43.119 (17)	Co—O2—O3	45.045 (13)
O1ⁱⁱⁱ—Co—O2ⁱⁱ	136.881 (17)	O1—O2—O3	117.10 (3)
O3—Co—O2ⁱⁱ	127.900 (13)	O1^v—O2—O3	116.45 (2)
O3ⁱ—Co—O2ⁱⁱ	52.099 (13)	O2^v—O2—O3	66.779 (11)
O2—Co—O2ⁱⁱⁱ	98.301 (14)	O3^ix—O2—O3	125.60 (2)
O2ⁱ—Co—O2ⁱⁱⁱ	81.699 (14)	O1ⁱⁱⁱ—O2—O3	63.366 (18)
O1ⁱⁱ—Co—O2ⁱⁱⁱ	136.881 (17)	O3ⁱ—O2—O3	93.353 (17)
O1ⁱⁱⁱ—Co—O2ⁱⁱⁱ	43.119 (17)	O1ⁱⁱ—O2—O3	56.821 (14)
O3—Co—O2ⁱⁱⁱ	52.100 (13)	S—O2—O1^xii	96.69 (3)
O3ⁱ—Co—O2ⁱⁱⁱ	127.901 (13)	Co—O2—O1^xii	112.81 (2)
O2ⁱⁱ—Co—O2ⁱⁱⁱ	180.000 (18)	O1—O2—O1^xii	85.159 (18)
O2—Co—O2^iv	137.542 (18)	O1^v—O2—O1^xii	73.82 (2)
O2ⁱ—Co—O2^iv	42.458 (19)	O2^v—O2—O1^xii	131.020 (16)
O1ⁱⁱ—Co—O2^iv	112.43 (2)	O3^ix—O2—O1^xii	57.343 (18)
O1ⁱⁱⁱ—Co—O2^iv	67.57 (2)	O1ⁱⁱⁱ—O2—O1^xii	100.90 (2)
O3—Co—O2^iv	119.74 (2)	O3ⁱ—O2—O1^xii	64.56 (2)
O3ⁱ—Co—O2^iv	60.26 (2)	O1ⁱⁱ—O2—O1^xii	110.66 (2)
O2ⁱⁱ—Co—O2^iv	95.775 (16)	O3—O2—O1^xii	157.73 (2)
O2ⁱⁱⁱ—Co—O2^iv	84.225 (16)	S—O2—O1^vii	81.81 (2)
O2—Co—O2^v	42.458 (18)	Co—O2—O1^vii	94.37 (2)
O2ⁱ—Co—O2^v	137.542 (19)	O1—O2—O1^vii	71.86 (3)
O1ⁱⁱ—Co—O2^v	67.57 (2)	O1^v—O2—O1^vii	115.94 (3)
O1ⁱⁱⁱ—Co—O2^v	112.43 (2)	O2^v—O2—O1^vii	61.13 (2)
O3—Co—O2^v	60.26 (2)	O3^ix—O2—O1^vii	87.10 (2)
O3ⁱ—Co—O2^v	119.74 (2)	O1ⁱⁱⁱ—O2—O1^vii	78.111 (18)
O2ⁱⁱ—Co—O2^v	84.225 (17)	O3ⁱ—O2—O1^vii	136.95 (2)
O2ⁱⁱⁱ—Co—O2^v	95.775 (16)	O1ⁱⁱ—O2—O1^vii	107.10 (2)
O2^iv—Co—O2^v	180.000 (10)	O3—O2—O1^vii	53.791 (13)
O1—S—O1^v	109.87 (5)	O1^xii—O2—O1^vii	142.23 (2)
O1—S—O2	108.72 (3)	Co—O3—Co^v	122.23 (3)
O1^v—S—O2	110.06 (3)	Co—O3—O2^xiii	111.681 (15)
O1—S—O2^v	110.06 (3)	Co^v—O3—O2^xiii	88.694 (14)
O1^v—S—O2^v	108.72 (3)	Co—O3—O2ⁱⁱⁱ	88.694 (13)
O2—S—O2^v	109.41 (4)	Co^v—O3—O2ⁱⁱⁱ	111.681 (15)
S—O1—Co^vi	136.87 (3)	O2^xiii—O3—O2ⁱⁱⁱ	137.95 (4)
S—O1—O2	35.890 (18)	Co—O3—O1ⁱⁱ	45.071 (14)
Co^vi—O1—O2	101.01 (3)	Co^v—O3—O1ⁱⁱ	104.28 (3)
S—O1—O1^v	35.07 (2)	O2^xiii—O3—O1ⁱⁱ	70.509 (19)
Co^vi—O1—O1^v	141.25 (4)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	132.459 (17)
O2—O1—O1^v	60.52 (2)	Co—O3—O1^vii	104.28 (3)
S—O1—O2^v	35.211 (19)	Co^v—O3—O1^vii	45.071 (14)
Co^vi—O1—O2^v	143.97 (3)	O2^xiii—O3—O1^vii	132.459 (17)
O2—O1—O2^v	60.41 (3)	O2ⁱⁱⁱ—O3—O1^vii	70.509 (19)
O1^v—O1—O2^v	59.69 (2)	O1ⁱⁱ—O3—O1^vii	123.18 (4)
S—O1—O2^vi	129.07 (3)	Co—O3—O2^xiv	161.58 (3)
Co^vi—O1—O2^vi	47.219 (16)	Co^v—O3—O2^xiv	44.775 (13)
O2—O1—O2^vi	110.06 (2)	O2^xiii—O3—O2^xiv	83.357 (18)
O1^v—O1—O2^vi	103.99 (3)	O2ⁱⁱⁱ—O3—O2^xiv	86.460 (19)
O2^v—O1—O2^vi	163.33 (3)	O1ⁱⁱ—O3—O2^xiv	140.733 (18)
S—O1—O3^vii	169.38 (4)	O1^vii—O3—O2^xiv	57.389 (17)
Co^vi—O1—O3^vii	48.572 (13)	Co—O3—O2ⁱ	44.775 (13)
O2—O1—O3^vii	147.05 (3)	Co^v—O3—O2ⁱ	161.58 (3)
O1^v—O1—O3^vii	150.097 (19)	O2^xiii—O3—O2ⁱ	86.460 (19)
O2^v—O1—O3^vii	134.22 (3)	O2ⁱⁱⁱ—O3—O2ⁱ	83.357 (18)
O2^vi—O1—O3^vii	61.549 (19)	O1ⁱⁱ—O3—O2ⁱ	57.389 (17)
S—O1—O2^viii	114.32 (3)	O1^vii—O3—O2ⁱ	140.733 (18)
Co^vi—O1—O2^viii	42.719 (16)	O2^xiv—O3—O2ⁱ	151.37 (3)
O2—O1—O2^viii	86.74 (2)	Co—O3—O2	41.873 (15)
O1^v—O1—O2^viii	147.05 (2)	Co^v—O3—O2	81.77 (2)
O2^v—O1—O2^viii	102.50 (3)	O2^xiii—O3—O2	125.60 (2)
O2^vi—O1—O2^viii	89.94 (2)	O2ⁱⁱⁱ—O3—O2	94.435 (15)
O3^vii—O1—O2^viii	62.54 (2)	O1ⁱⁱ—O3—O2	60.64 (2)
S—O1—O3^ix	92.83 (3)	O1^vii—O3—O2	67.41 (2)
Co^vi—O1—O3^ix	44.721 (14)	O2^xiv—O3—O2	120.86 (2)
O2—O1—O3^ix	57.77 (2)	O2ⁱ—O3—O2	86.647 (17)
O1^v—O1—O3^ix	103.00 (3)	Co—O3—O2^v	81.77 (2)
O2^v—O1—O3^ix	114.98 (3)	Co^v—O3—O2^v	41.873 (15)
O2^vi—O1—O3^ix	62.79 (2)	O2^xiii—O3—O2^v	94.435 (15)
O3^vii—O1—O3^ix	93.29 (2)	O2ⁱⁱⁱ—O3—O2^v	125.60 (2)
O2^viii—O1—O3^ix	56.945 (17)	O1ⁱⁱ—O3—O2^v	67.41 (2)
S—O1—O2^x	125.28 (3)	O1^vii—O3—O2^v	60.64 (2)
Co^vi—O1—O2^x	97.51 (2)	O2^xiv—O3—O2^v	86.647 (17)
O2—O1—O2^x	160.77 (3)	O2ⁱ—O3—O2^v	120.86 (2)
O1^v—O1—O2^x	101.33 (2)	O2—O3—O2^v	46.44 (2)
O2^v—O1—O2^x	106.18 (2)	Co—O3—O1^xiii	121.38 (2)
O2^vi—O1—O2^x	79.10 (2)	Co^v—O3—O1^xiii	41.637 (11)
O3^vii—O1—O2^x	52.147 (16)	O2^xiii—O3—O1^xiii	48.267 (15)
O2^viii—O1—O2^x	110.66 (2)	O2ⁱⁱⁱ—O3—O1^xiii	146.519 (17)
O3^ix—O1—O2^x	138.58 (2)	O1ⁱⁱ—O3—O1^xiii	80.451 (18)
S—O1—O3^xi	103.74 (3)	O1^vii—O3—O1^xiii	86.71 (2)
Co^vi—O1—O3^xi	97.79 (2)	O2^xiv—O3—O1^xiii	60.313 (17)
O2—O1—O3^xi	118.78 (3)	O2ⁱ—O3—O1^xiii	127.685 (17)
O1^v—O1—O3^xi	68.671 (11)	O2—O3—O1^xiii	99.13 (2)
O2^v—O1—O3^xi	118.12 (2)	O2^v—O3—O1^xiii	53.846 (16)
O2^vi—O1—O3^xi	52.201 (17)	Co—O3—O1ⁱⁱⁱ	41.637 (12)
O3^vii—O1—O3^xi	82.652 (18)	Co^v—O3—O1ⁱⁱⁱ	121.38 (2)
O2^viii—O1—O3^xi	138.69 (2)	O2^xiii—O3—O1ⁱⁱⁱ	146.519 (17)
O3^ix—O1—O3^xi	107.48 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	48.267 (16)
O2^x—O1—O3^xi	52.821 (15)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	86.71 (2)
S—O1—O2^vii	111.40 (3)	O1^vii—O3—O1ⁱⁱⁱ	80.451 (18)
Co^vi—O1—O2^vii	77.47 (2)	O2^xiv—O3—O1ⁱⁱⁱ	127.685 (17)
O2—O1—O2^vii	108.14 (3)	O2ⁱ—O3—O1ⁱⁱⁱ	60.313 (17)
O1^v—O1—O2^vii	138.73 (3)	O2—O3—O1ⁱⁱⁱ	53.846 (16)
O2^v—O1—O2^vii	79.91 (2)	O2^v—O3—O1ⁱⁱⁱ	99.13 (2)
O2^vi—O1—O2^vii	116.71 (2)	O1^xiii—O3—O1ⁱⁱⁱ	152.85 (3)
O3^vii—O1—O2^vii	58.80 (2)	Co—O3—H	107.2 (12)
O2^viii—O1—O2^vii	44.668 (19)	Co^v—O3—H	107.6 (11)
O3^ix—O1—O2^vii	101.37 (2)	O2^xiii—O3—H	119.4 (11)
O2^x—O1—O2^vii	80.888 (17)	O2ⁱⁱⁱ—O3—H	20.8 (12)
O3^xi—O1—O2^vii	132.778 (18)	O1ⁱⁱ—O3—H	146.6 (11)
S—O2—Co	132.61 (3)	O1^vii—O3—H	75.7 (11)
S—O2—O1	35.395 (18)	O2^xiv—O3—H	72.0 (12)
Co—O2—O1	161.53 (3)	O2ⁱ—O3—H	90.2 (11)
S—O2—O1^v	34.730 (18)	O2—O3—H	114.5 (12)
Co—O2—O1^v	119.45 (3)	O2^v—O3—H	136.2 (11)
O1—O2—O1^v	59.80 (3)	O1^xiii—O3—H	131.1 (12)
S—O2—O2^v	35.29 (2)	O1ⁱⁱⁱ—O3—H	68.4 (12)
Co—O2—O2^v	102.637 (19)	Co—O3—H^v	107.6 (11)
O1—O2—O2^v	60.20 (2)	Co^v—O3—H^v	107.2 (12)
O1^v—O2—O2^v	59.39 (2)	O2^xiii—O3—H^v	20.8 (12)
S—O2—O3^ix	108.37 (3)	O2ⁱⁱⁱ—O3—H^v	119.4 (12)
Co—O2—O3^ix	118.63 (2)	O1ⁱⁱ—O3—H^v	75.7 (11)
O1—O2—O3^ix	73.96 (2)	O1^vii—O3—H^v	146.6 (11)
O1^v—O2—O3^ix	114.26 (3)	O2^xiv—O3—H^v	90.2 (11)
O2^v—O2—O3^ix	129.81 (3)	O2ⁱ—O3—H^v	72.0 (12)
S—O2—O1ⁱⁱⁱ	159.72 (3)	O2—O3—H^v	136.2 (11)
Co—O2—O1ⁱⁱⁱ	47.287 (17)	O2^v—O3—H^v	114.5 (12)
O1—O2—O1ⁱⁱⁱ	136.37 (2)	O1^xiii—O3—H^v	68.4 (12)
O1^v—O2—O1ⁱⁱⁱ	163.33 (3)	O1ⁱⁱⁱ—O3—H^v	131.1 (12)
O2^v—O2—O1ⁱⁱⁱ	128.073 (18)	H—O3—H^v	104 (2)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x, −y+1, z−1/2; (v) −x, y, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) x, y−1, z; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.797 (15)	1.993 (15)	2.7186 (7)	151.1 (16)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(CoSO4H2O_N2_313K) top

Crystal data top

CoH₂O₅S	V = 355.03 (9) Å³
M_r = 173.01	Z = 4
Monoclinic, C2/c	F(000) = 340
a = 6.9765 (10) Å	D_x = 3.237 Mg m⁻³
b = 7.5904 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.6373 (10) Å	µ = 5.30 mm⁻¹
β = 118.616 (10)°	T = 313 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.020
T_min = 0.583, T_max = 0.748	θ_max = 40.0°, θ_min = 4.2°
11538 measured reflections	h = −12→12
1105 independent reflections	k = −13→13
1094 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.012	w = 1/[σ²(F_o²) + (0.014P)² + 0.2P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.033	(Δ/σ)_max < 0.001
S = 1.21	Δρ_max = 0.44 e Å⁻³
1105 reflections	Δρ_min = −0.41 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0239 (11)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co	0.000000	0.500000	0.000000	0.00773 (4)
S	0.000000	0.15349 (3)	0.250000	0.00676 (4)
O1	0.17268 (8)	0.04243 (8)	0.39981 (8)	0.01420 (9)
O2	0.09640 (8)	0.26637 (7)	0.15370 (8)	0.01236 (8)
O3	0.000000	0.63871 (10)	0.250000	0.01098 (10)
H	0.101 (2)	0.704 (2)	0.295 (2)	0.031 (4)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co	0.00722 (5)	0.00778 (5)	0.00821 (5)	−0.00010 (3)	0.00373 (4)	0.00052 (3)
S	0.00542 (7)	0.00632 (7)	0.00835 (7)	0.000	0.00315 (5)	0.000
O1	0.00875 (17)	0.0160 (2)	0.0166 (2)	0.00400 (15)	0.00506 (15)	0.00796 (17)
O2	0.01246 (18)	0.01089 (18)	0.01701 (19)	0.00190 (14)	0.00970 (16)	0.00524 (15)
O3	0.0112 (2)	0.0117 (3)	0.0108 (2)	0.000	0.0058 (2)	0.000

Geometric parameters (Å, º) top

Co—O2ⁱ	2.0540 (5)	O1—O1^iv	2.4001 (11)
Co—O2	2.0540 (5)	O1—O2^iv	2.4177 (8)
Co—O1ⁱⁱ	2.0567 (6)	O1—O2^vi	2.7900 (8)
Co—O1ⁱⁱⁱ	2.0567 (6)	O1—O3^vii	2.8997 (7)
Co—O3ⁱ	2.1804 (4)	O1—O2^viii	3.0190 (9)
Co—O3	2.1804 (4)	O1—O3^ix	3.0920 (7)
Co—O2ⁱⁱⁱ	3.4464 (6)	O1—O2^x	3.2442 (8)
Co—O2ⁱⁱ	3.4464 (7)	O1—O3^xi	3.2910 (10)
Co—O2^iv	3.5066 (6)	O1—O2^vii	3.3268 (9)
Co—O2^v	3.5066 (6)	O2—O2^iv	2.4225 (10)
S—O1	1.4665 (5)	O2—O3^ix	2.7248 (7)
S—O1^iv	1.4665 (5)	O2—O3ⁱ	2.9140 (7)
S—O2	1.4836 (5)	O2—O3	3.0749 (9)
S—O2^iv	1.4836 (5)	O3—H	0.796 (16)
O1—O2	2.3974 (7)	O3—H^iv	0.796 (16)

O2ⁱ—Co—O2	180.0	O3^ix—O2—O1ⁱⁱⁱ	73.27 (2)
O2ⁱ—Co—O1ⁱⁱ	85.48 (2)	S—O2—O3ⁱ	137.53 (3)
O2—Co—O1ⁱⁱ	94.52 (2)	Co—O2—O3ⁱ	48.346 (17)
O2ⁱ—Co—O1ⁱⁱⁱ	94.52 (2)	O1—O2—O3ⁱ	148.98 (3)
O2—Co—O1ⁱⁱⁱ	85.48 (2)	O1^iv—O2—O3ⁱ	103.18 (3)
O1ⁱⁱ—Co—O1ⁱⁱⁱ	180.0	O2^iv—O2—O3ⁱ	136.77 (3)
O2ⁱ—Co—O3ⁱ	93.08 (2)	O3^ix—O2—O3ⁱ	93.36 (2)
O2—Co—O3ⁱ	86.92 (2)	O1ⁱⁱⁱ—O2—O3ⁱ	61.064 (19)
O1ⁱⁱ—Co—O3ⁱ	93.684 (18)	S—O2—O1ⁱⁱ	93.39 (3)
O1ⁱⁱⁱ—Co—O3ⁱ	86.316 (18)	Co—O2—O1ⁱⁱ	42.778 (15)
O2ⁱ—Co—O3	86.92 (2)	O1—O2—O1ⁱⁱ	128.74 (3)
O2—Co—O3	93.08 (2)	O1^iv—O2—O1ⁱⁱ	77.72 (3)
O1ⁱⁱ—Co—O3	86.316 (18)	O2^iv—O2—O1ⁱⁱ	74.48 (3)
O1ⁱⁱⁱ—Co—O3	93.684 (18)	O3^ix—O2—O1ⁱⁱ	155.74 (2)
O3ⁱ—Co—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.08 (2)
O2ⁱ—Co—O2ⁱⁱⁱ	81.698 (14)	O3ⁱ—O2—O1ⁱⁱ	62.791 (18)
O2—Co—O2ⁱⁱⁱ	98.301 (14)	S—O2—O3	102.08 (3)
O1ⁱⁱ—Co—O2ⁱⁱⁱ	136.955 (18)	Co—O2—O3	45.078 (14)
O1ⁱⁱⁱ—Co—O2ⁱⁱⁱ	43.045 (18)	O1—O2—O3	117.13 (3)
O3ⁱ—Co—O2ⁱⁱⁱ	127.781 (13)	O1^iv—O2—O3	116.46 (2)
O3—Co—O2ⁱⁱⁱ	52.219 (13)	O2^iv—O2—O3	66.802 (11)
O2ⁱ—Co—O2ⁱⁱ	98.302 (13)	O3^ix—O2—O3	125.34 (2)
O2—Co—O2ⁱⁱ	81.699 (13)	O1ⁱⁱⁱ—O2—O3	63.416 (18)
O1ⁱⁱ—Co—O2ⁱⁱ	43.045 (18)	O3ⁱ—O2—O3	93.424 (18)
O1ⁱⁱⁱ—Co—O2ⁱⁱ	136.955 (18)	O1ⁱⁱ—O2—O3	56.818 (15)
O3ⁱ—Co—O2ⁱⁱ	52.219 (13)	S—O2—O1^xii	97.01 (3)
O3—Co—O2ⁱⁱ	127.781 (13)	Co—O2—O1^xii	112.63 (2)
O2ⁱⁱⁱ—Co—O2ⁱⁱ	180.0	O1—O2—O1^xii	85.298 (19)
O2ⁱ—Co—O2^iv	137.655 (19)	O1^iv—O2—O1^xii	74.18 (2)
O2—Co—O2^iv	42.345 (19)	O2^iv—O2—O1^xii	131.350 (17)
O1ⁱⁱ—Co—O2^iv	67.76 (2)	O3^ix—O2—O1^xii	57.338 (18)
O1ⁱⁱⁱ—Co—O2^iv	112.24 (2)	O1ⁱⁱⁱ—O2—O1^xii	100.58 (2)
O3ⁱ—Co—O2^iv	119.78 (2)	O3ⁱ—O2—O1^xii	64.35 (2)
O3—Co—O2^iv	60.22 (2)	O1ⁱⁱ—O2—O1^xii	110.73 (2)
O2ⁱⁱⁱ—Co—O2^iv	95.693 (16)	O3—O2—O1^xii	157.56 (2)
O2ⁱⁱ—Co—O2^iv	84.308 (16)	S—O2—O1^vii	81.71 (3)
O2ⁱ—Co—O2^v	42.345 (19)	Co—O2—O1^vii	94.27 (2)
O2—Co—O2^v	137.655 (19)	O1—O2—O1^vii	71.88 (3)
O1ⁱⁱ—Co—O2^v	112.24 (2)	O1^iv—O2—O1^vii	115.82 (3)
O1ⁱⁱⁱ—Co—O2^v	67.76 (2)	O2^iv—O2—O1^vii	60.97 (2)
O3ⁱ—Co—O2^v	60.22 (2)	O3^ix—O2—O1^vii	87.02 (2)
O3—Co—O2^v	119.78 (2)	O1ⁱⁱⁱ—O2—O1^vii	78.015 (18)
O2ⁱⁱⁱ—Co—O2^v	84.307 (16)	O3ⁱ—O2—O1^vii	136.86 (2)
O2ⁱⁱ—Co—O2^v	95.692 (16)	O1ⁱⁱ—O2—O1^vii	107.05 (2)
O2^iv—Co—O2^v	180.000 (15)	O3—O2—O1^vii	53.691 (14)
O1—S—O1^iv	109.83 (5)	O1^xii—O2—O1^vii	142.21 (2)
O1—S—O2	108.71 (3)	Co—O3—Co^iv	122.25 (3)
O1^iv—S—O2	110.07 (3)	Co—O3—O2ⁱⁱⁱ	88.550 (14)
O1—S—O2^iv	110.07 (3)	Co^iv—O3—O2ⁱⁱⁱ	111.638 (15)
O1^iv—S—O2^iv	108.71 (3)	Co—O3—O2^xiii	111.637 (15)
O2—S—O2^iv	109.45 (4)	Co^iv—O3—O2^xiii	88.551 (14)
S—O1—Co^vi	136.98 (3)	O2ⁱⁱⁱ—O3—O2^xiii	138.34 (4)
S—O1—O2	35.885 (18)	Co—O3—O1ⁱⁱ	45.059 (15)
Co^vi—O1—O2	101.11 (3)	Co^iv—O3—O1ⁱⁱ	104.38 (3)
S—O1—O1^iv	35.09 (3)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	132.307 (18)
Co^vi—O1—O1^iv	141.58 (4)	O2^xiii—O3—O1ⁱⁱ	70.374 (19)
O2—O1—O1^iv	60.52 (2)	Co—O3—O1^vii	104.38 (3)
S—O1—O2^iv	35.197 (19)	Co^iv—O3—O1^vii	45.060 (15)
Co^vi—O1—O2^iv	143.79 (3)	O2ⁱⁱⁱ—O3—O1^vii	70.374 (19)
O2—O1—O2^iv	60.41 (3)	O2^xiii—O3—O1^vii	132.308 (17)
O1^iv—O1—O2^iv	59.68 (2)	O1ⁱⁱ—O3—O1^vii	123.39 (4)
S—O1—O2^vi	129.32 (4)	Co—O3—O2^xiv	161.65 (3)
Co^vi—O1—O2^vi	47.216 (16)	Co^iv—O3—O2^xiv	44.738 (13)
O2—O1—O2^vi	110.16 (2)	O2ⁱⁱⁱ—O3—O2^xiv	86.64 (2)
O1^iv—O1—O2^vi	104.29 (3)	O2^xiii—O3—O2^xiv	83.263 (18)
O2^iv—O1—O2^vi	163.61 (3)	O1ⁱⁱ—O3—O2^xiv	140.704 (18)
S—O1—O3^vii	169.10 (4)	O1^vii—O3—O2^xiv	57.357 (18)
Co^vi—O1—O3^vii	48.624 (13)	Co—O3—O2ⁱ	44.738 (13)
O2—O1—O3^vii	147.18 (3)	Co^iv—O3—O2ⁱ	161.65 (3)
O1^iv—O1—O3^vii	150.10 (2)	O2ⁱⁱⁱ—O3—O2ⁱ	83.263 (18)
O2^iv—O1—O3^vii	133.95 (3)	O2^xiii—O3—O2ⁱ	86.64 (2)
O2^vi—O1—O3^vii	61.578 (19)	O1ⁱⁱ—O3—O2ⁱ	57.357 (18)
S—O1—O2^viii	114.24 (3)	O1^vii—O3—O2ⁱ	140.704 (18)
Co^vi—O1—O2^viii	42.707 (16)	O2^xiv—O3—O2ⁱ	151.37 (4)
O2—O1—O2^viii	86.80 (2)	Co—O3—O2	41.838 (15)
O1^iv—O1—O2^viii	147.08 (2)	Co^iv—O3—O2	81.80 (2)
O2^iv—O1—O2^viii	102.28 (3)	O2ⁱⁱⁱ—O3—O2	94.318 (15)
O2^vi—O1—O2^viii	89.92 (2)	O2^xiii—O3—O2	125.34 (2)
O3^vii—O1—O2^viii	62.56 (2)	O1ⁱⁱ—O3—O2	60.62 (2)
S—O1—O3^ix	92.97 (3)	O1^vii—O3—O2	67.60 (2)
Co^vi—O1—O3^ix	44.725 (14)	O2^xiv—O3—O2	120.95 (2)
O2—O1—O3^ix	57.88 (2)	O2ⁱ—O3—O2	86.576 (18)
O1^iv—O1—O3^ix	103.25 (3)	Co—O3—O2^iv	81.80 (2)
O2^iv—O1—O3^ix	114.99 (3)	Co^iv—O3—O2^iv	41.838 (15)
O2^vi—O1—O3^ix	62.79 (2)	O2ⁱⁱⁱ—O3—O2^iv	125.34 (3)
O3^vii—O1—O3^ix	93.35 (2)	O2^xiii—O3—O2^iv	94.318 (15)
O2^viii—O1—O3^ix	56.943 (17)	O1ⁱⁱ—O3—O2^iv	67.60 (2)
S—O1—O2^x	124.96 (3)	O1^vii—O3—O2^iv	60.62 (2)
Co^vi—O1—O2^x	97.77 (2)	O2^xiv—O3—O2^iv	86.575 (18)
O2—O1—O2^x	160.48 (3)	O2ⁱ—O3—O2^iv	120.95 (2)
O1^iv—O1—O2^x	101.11 (2)	O2—O3—O2^iv	46.40 (2)
O2^iv—O1—O2^x	105.82 (2)	Co—O3—O1^xiii	121.31 (2)
O2^vi—O1—O2^x	79.42 (2)	Co^iv—O3—O1^xiii	41.591 (12)
O3^vii—O1—O2^x	52.288 (17)	O2ⁱⁱⁱ—O3—O1^xiii	146.618 (17)
O2^viii—O1—O2^x	110.73 (2)	O2^xiii—O3—O1^xiii	48.171 (16)
O3^ix—O1—O2^x	138.90 (2)	O1ⁱⁱ—O3—O1^xiii	80.461 (18)
S—O1—O3^xi	103.70 (3)	O1^vii—O3—O1^xiii	86.65 (2)
Co^vi—O1—O3^xi	98.04 (2)	O2^xiv—O3—O1^xiii	60.266 (17)
O2—O1—O3^xi	118.74 (3)	O2ⁱ—O3—O1^xiii	127.796 (17)
O1^iv—O1—O3^xi	68.614 (11)	O2—O3—O1^xiii	98.98 (2)
O2^iv—O1—O3^xi	118.07 (2)	O2^iv—O3—O1^xiii	53.796 (16)
O2^vi—O1—O3^xi	52.456 (17)	Co—O3—O1ⁱⁱⁱ	41.591 (11)
O3^vii—O1—O3^xi	82.796 (19)	Co^iv—O3—O1ⁱⁱⁱ	121.31 (2)
O2^viii—O1—O3^xi	138.91 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	48.171 (16)
O3^ix—O1—O3^xi	107.68 (2)	O2^xiii—O3—O1ⁱⁱⁱ	146.617 (17)
O2^x—O1—O3^xi	52.954 (15)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	86.65 (2)
S—O1—O2^vii	111.26 (3)	O1^vii—O3—O1ⁱⁱⁱ	80.461 (18)
Co^vi—O1—O2^vii	77.33 (2)	O2^xiv—O3—O1ⁱⁱⁱ	127.796 (17)
O2—O1—O2^vii	108.12 (3)	O2ⁱ—O3—O1ⁱⁱⁱ	60.266 (17)
O1^iv—O1—O2^vii	138.55 (3)	O2—O3—O1ⁱⁱⁱ	53.796 (16)
O2^iv—O1—O2^vii	79.76 (2)	O2^iv—O3—O1ⁱⁱⁱ	98.98 (2)
O2^vi—O1—O2^vii	116.59 (2)	O1^xiii—O3—O1ⁱⁱⁱ	152.66 (3)
O3^vii—O1—O2^vii	58.71 (2)	Co—O3—H	108.1 (12)
O2^viii—O1—O2^vii	44.555 (19)	Co^iv—O3—H	107.1 (11)
O3^ix—O1—O2^vii	101.26 (2)	O2ⁱⁱⁱ—O3—H	21.9 (12)
O2^x—O1—O2^vii	80.799 (17)	O2^xiii—O3—H	118.9 (12)
O3^xi—O1—O2^vii	132.805 (19)	O1ⁱⁱ—O3—H	147.3 (12)
S—O2—Co	132.83 (3)	O1^vii—O3—H	75.6 (11)
S—O2—O1	35.409 (18)	O2^xiv—O3—H	71.2 (12)
Co—O2—O1	161.66 (3)	O2ⁱ—O3—H	90.7 (12)
S—O2—O1^iv	34.731 (19)	O2—O3—H	115.4 (12)
Co—O2—O1^iv	119.68 (3)	O2^iv—O3—H	136.2 (11)
O1—O2—O1^iv	59.79 (3)	O1^xiii—O3—H	130.3 (12)
S—O2—O2^iv	35.27 (2)	O1ⁱⁱⁱ—O3—H	69.5 (12)
Co—O2—O2^iv	102.825 (19)	Co—O3—H^iv	107.1 (11)
O1—O2—O2^iv	60.21 (2)	Co^iv—O3—H^iv	108.1 (12)
O1^iv—O2—O2^iv	59.38 (2)	O2ⁱⁱⁱ—O3—H^iv	118.9 (12)
S—O2—O3^ix	108.42 (3)	O2^xiii—O3—H^iv	21.9 (12)
Co—O2—O3^ix	118.33 (2)	O1ⁱⁱ—O3—H^iv	75.6 (11)
O1—O2—O3^ix	73.95 (2)	O1^vii—O3—H^iv	147.3 (12)
O1^iv—O2—O3^ix	114.45 (3)	O2^xiv—O3—H^iv	90.7 (12)
O2^iv—O2—O3^ix	129.69 (3)	O2ⁱ—O3—H^iv	71.2 (12)
S—O2—O1ⁱⁱⁱ	159.55 (3)	O2—O3—H^iv	136.2 (11)
Co—O2—O1ⁱⁱⁱ	47.300 (18)	O2^iv—O3—H^iv	115.4 (12)
O1—O2—O1ⁱⁱⁱ	136.09 (2)	O1^xiii—O3—H^iv	69.5 (12)
O1^iv—O2—O1ⁱⁱⁱ	163.61 (3)	O1ⁱⁱⁱ—O3—H^iv	130.3 (12)
O2^iv—O2—O1ⁱⁱⁱ	128.057 (19)	H—O3—H^iv	103 (2)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x, y, −z+1/2; (v) x, −y+1, z−1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) x, y−1, z; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.796 (16)	2.008 (15)	2.7248 (7)	149.6 (16)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(NiSO4H2O_He_15K) top

Crystal data top

H₂NiO₅S	V = 343.15 (10) Å³
M_r = 172.79	Z = 4
Monoclinic, C2/c	F(000) = 344
a = 6.7979 (11) Å	D_x = 3.345 Mg m⁻³
b = 7.6403 (9) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.4489 (12) Å	µ = 6.14 mm⁻¹
β = 117.51 (2)°	T = 15 K

Data collection top

1157 measured reflections	θ_max = 29.4°, θ_min = 4.3°
430 independent reflections	h = −5→9
398 reflections with I > 2σ(I)	k = −9→10
R_int = 0.036	l = −10→8

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.026	w = 1/[σ²(F_o²) + (0.035P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.066	(Δ/σ)_max < 0.001
S = 1.11	Δρ_max = 0.88 e Å⁻³
430 reflections	Δρ_min = −0.66 e Å⁻³
40 parameters	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.033 (3)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ni	0.000000	0.500000	0.000000	0.0077 (2)
S	0.000000	0.15772 (12)	0.250000	0.0078 (3)
O1	0.1727 (3)	0.0480 (3)	0.4050 (3)	0.0101 (4)
O2	0.1051 (3)	0.2710 (3)	0.1556 (2)	0.0085 (4)
O3	0.000000	0.6302 (4)	0.250000	0.0100 (6)
H	0.113 (6)	0.696 (5)	0.296 (5)	0.014 (9)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni	0.0073 (3)	0.0069 (3)	0.0093 (3)	−0.00018 (16)	0.0041 (2)	−0.00008 (14)
S	0.0075 (5)	0.0072 (5)	0.0092 (5)	0.000	0.0041 (4)	0.000
O1	0.0091 (11)	0.0093 (9)	0.0118 (9)	−0.0003 (8)	0.0047 (8)	0.0013 (7)
O2	0.0088 (10)	0.0082 (9)	0.0100 (9)	−0.0003 (7)	0.0056 (7)	0.0009 (7)
O3	0.0086 (15)	0.0099 (13)	0.0110 (13)	0.000	0.0040 (11)	0.000

Geometric parameters (Å, º) top

Ni—O1ⁱ	2.033 (2)	O1—O1^v	2.416 (4)
Ni—O1ⁱⁱ	2.033 (2)	O1—O2^v	2.426 (3)
Ni—O2ⁱⁱⁱ	2.0373 (19)	O1—O2^vi	2.756 (3)
Ni—O2	2.0373 (19)	O1—O3^vii	2.851 (2)
Ni—O3ⁱⁱⁱ	2.1111 (14)	O1—O2^viii	2.995 (3)
Ni—O3	2.1111 (14)	O1—O3^ix	3.009 (2)
Ni—O2ⁱ	3.422 (2)	O1—O2^vii	3.215 (3)
Ni—O2ⁱⁱ	3.422 (2)	O1—O2^x	3.229 (3)
Ni—O2^iv	3.4418 (17)	O1—O1^xi	3.335 (4)
Ni—O2^v	3.4418 (17)	O2—O2^v	2.424 (3)
S—O1^v	1.470 (2)	O2—O3^ix	2.667 (2)
S—O1	1.470 (2)	O2—O3ⁱⁱⁱ	2.8663 (18)
S—O2	1.4894 (18)	O2—O3	3.000 (3)
S—O2^v	1.4894 (18)	O3—H	0.84 (3)
O1—O2	2.404 (3)	O3—H^v	0.84 (3)

O1ⁱ—Ni—O1ⁱⁱ	180.0	O3^ix—O2—O1ⁱⁱ	78.00 (9)
O1ⁱ—Ni—O2ⁱⁱⁱ	85.23 (8)	S—O2—O3ⁱⁱⁱ	135.26 (10)
O1ⁱⁱ—Ni—O2ⁱⁱⁱ	94.77 (8)	Ni—O2—O3ⁱⁱⁱ	47.37 (6)
O1ⁱ—Ni—O2	94.77 (8)	O1—O2—O3ⁱⁱⁱ	150.13 (11)
O1ⁱⁱ—Ni—O2	85.23 (8)	O2^v—O2—O3ⁱⁱⁱ	133.21 (11)
O2ⁱⁱⁱ—Ni—O2	180.0	O1^v—O2—O3ⁱⁱⁱ	101.25 (8)
O1ⁱ—Ni—O3ⁱⁱⁱ	93.09 (6)	O3^ix—O2—O3ⁱⁱⁱ	96.59 (7)
O1ⁱⁱ—Ni—O3ⁱⁱⁱ	86.91 (6)	O1ⁱⁱ—O2—O3ⁱⁱⁱ	60.90 (7)
O2ⁱⁱⁱ—Ni—O3ⁱⁱⁱ	92.61 (8)	S—O2—O1ⁱ	90.89 (9)
O2—Ni—O3ⁱⁱⁱ	87.39 (8)	Ni—O2—O1ⁱ	42.56 (5)
O1ⁱ—Ni—O3	86.91 (6)	O1—O2—O1ⁱ	126.24 (10)
O1ⁱⁱ—Ni—O3	93.09 (6)	O2^v—O2—O1ⁱ	71.91 (8)
O2ⁱⁱⁱ—Ni—O3	87.39 (8)	O1^v—O2—O1ⁱ	75.68 (9)
O2—Ni—O3	92.61 (8)	O3^ix—O2—O1ⁱ	158.31 (7)
O3ⁱⁱⁱ—Ni—O3	180.00 (14)	O1ⁱⁱ—O2—O1ⁱ	89.87 (8)
O1ⁱ—Ni—O2ⁱ	43.65 (6)	O3ⁱⁱⁱ—O2—O1ⁱ	61.72 (6)
O1ⁱⁱ—Ni—O2ⁱ	136.35 (6)	S—O2—O3	101.70 (9)
O2ⁱⁱⁱ—Ni—O2ⁱ	98.37 (3)	Ni—O2—O3	44.67 (4)
O2—Ni—O2ⁱ	81.63 (3)	O1—O2—O3	116.64 (8)
O3ⁱⁱⁱ—Ni—O2ⁱ	51.20 (4)	O2^v—O2—O3	66.17 (4)
O3—Ni—O2ⁱ	128.80 (4)	O1^v—O2—O3	115.90 (9)
O1ⁱ—Ni—O2ⁱⁱ	136.35 (6)	O3^ix—O2—O3	128.83 (9)
O1ⁱⁱ—Ni—O2ⁱⁱ	43.65 (6)	O1ⁱⁱ—O2—O3	62.86 (6)
O2ⁱⁱⁱ—Ni—O2ⁱⁱ	81.64 (3)	O3ⁱⁱⁱ—O2—O3	92.04 (6)
O2—Ni—O2ⁱⁱ	98.37 (3)	O1ⁱ—O2—O3	56.78 (5)
O3ⁱⁱⁱ—Ni—O2ⁱⁱ	128.80 (4)	S—O2—O1^vii	82.63 (8)
O3—Ni—O2ⁱⁱ	51.20 (4)	Ni—O2—O1^vii	94.95 (7)
O2ⁱ—Ni—O2ⁱⁱ	180.00 (6)	O1—O2—O1^vii	71.69 (8)
O1ⁱ—Ni—O2^iv	113.77 (6)	O2^v—O2—O1^vii	62.31 (7)
O1ⁱⁱ—Ni—O2^iv	66.23 (6)	O1^v—O2—O1^vii	116.80 (9)
O2ⁱⁱⁱ—Ni—O2^iv	43.81 (7)	O3^ix—O2—O1^vii	87.87 (7)
O2—Ni—O2^iv	136.19 (7)	O1ⁱⁱ—O2—O1^vii	78.53 (6)
O3ⁱⁱⁱ—Ni—O2^iv	59.83 (7)	O3ⁱⁱⁱ—O2—O1^vii	136.96 (9)
O3—Ni—O2^iv	120.17 (7)	O1ⁱ—O2—O1^vii	107.47 (8)
O2ⁱ—Ni—O2^iv	96.31 (4)	O3—O2—O1^vii	54.47 (5)
O2ⁱⁱ—Ni—O2^iv	83.69 (4)	S—O2—O1^xii	93.53 (9)
O1ⁱ—Ni—O2^v	66.23 (6)	Ni—O2—O1^xii	115.18 (7)
O1ⁱⁱ—Ni—O2^v	113.77 (6)	O1—O2—O1^xii	83.36 (6)
O2ⁱⁱⁱ—Ni—O2^v	136.19 (7)	O2^v—O2—O1^xii	127.92 (6)
O2—Ni—O2^v	43.81 (7)	O1^v—O2—O1^xii	70.64 (8)
O3ⁱⁱⁱ—Ni—O2^v	120.17 (7)	O3^ix—O2—O1^xii	56.87 (6)
O3—Ni—O2^v	59.83 (7)	O1ⁱⁱ—O2—O1^xii	104.47 (7)
O2ⁱ—Ni—O2^v	83.69 (4)	O3ⁱⁱⁱ—O2—O1^xii	67.81 (7)
O2ⁱⁱ—Ni—O2^v	96.31 (4)	O1ⁱ—O2—O1^xii	110.42 (8)
O2^iv—Ni—O2^v	180.00 (3)	O3—O2—O1^xii	159.85 (7)
O1^v—S—O1	110.48 (17)	O1^vii—O2—O1^xii	141.97 (7)
O1^v—S—O2	110.10 (10)	Ni—O3—Ni^v	123.80 (14)
O1—S—O2	108.60 (11)	Ni—O3—O2^xiii	111.56 (4)
O1^v—S—O2^v	108.60 (11)	Ni^v—O3—O2^xiii	90.72 (4)
O1—S—O2^v	110.10 (10)	Ni—O3—O2ⁱⁱ	90.72 (4)
O2—S—O2^v	108.94 (16)	Ni^v—O3—O2ⁱⁱ	111.56 (4)
S—O1—Ni^vi	136.44 (12)	O2^xiii—O3—O2ⁱⁱ	132.41 (14)
S—O1—O2	35.97 (7)	Ni—O3—O1ⁱ	45.40 (5)
Ni^vi—O1—O2	100.63 (9)	Ni^v—O3—O1ⁱ	104.61 (9)
S—O1—O1^v	34.76 (9)	O2^xiii—O3—O1ⁱ	71.55 (6)
Ni^vi—O1—O1^v	139.19 (13)	O2ⁱⁱ—O3—O1ⁱ	134.57 (5)
O2—O1—O1^v	60.45 (7)	Ni—O3—O1^vii	104.61 (9)
S—O1—O2^v	35.21 (6)	Ni^v—O3—O1^vii	45.40 (5)
Ni^vi—O1—O2^v	145.52 (12)	O2^xiii—O3—O1^vii	134.57 (5)
O2—O1—O2^v	60.26 (9)	O2ⁱⁱ—O3—O1^vii	71.55 (6)
O1^v—O1—O2^v	59.52 (8)	O1ⁱ—O3—O1^vii	122.96 (13)
S—O1—O2^vi	127.47 (11)	Ni—O3—O2^xiv	162.25 (9)
Ni^vi—O1—O2^vi	47.45 (6)	Ni^v—O3—O2^xiv	45.24 (4)
O2—O1—O2^vi	109.95 (7)	O2^xiii—O3—O2^xiv	84.39 (6)
O1^v—O1—O2^vi	101.97 (8)	O2ⁱⁱ—O3—O2^xiv	83.41 (7)
O2^v—O1—O2^vi	161.31 (11)	O1ⁱ—O3—O2^xiv	141.90 (7)
S—O1—O3^vii	171.06 (12)	O1^vii—O3—O2^xiv	57.64 (6)
Ni^vi—O1—O3^vii	47.69 (4)	Ni—O3—O2ⁱⁱⁱ	45.24 (4)
O2—O1—O3^vii	145.71 (10)	Ni^v—O3—O2ⁱⁱⁱ	162.25 (9)
O1^v—O1—O3^vii	150.58 (7)	O2^xiii—O3—O2ⁱⁱⁱ	83.41 (7)
O2^v—O1—O3^vii	136.02 (9)	O2ⁱⁱ—O3—O2ⁱⁱⁱ	84.39 (6)
O2^vi—O1—O3^vii	61.47 (7)	O1ⁱ—O3—O2ⁱⁱⁱ	57.64 (6)
S—O1—O2^viii	115.09 (11)	O1^vii—O3—O2ⁱⁱⁱ	141.90 (7)
Ni^vi—O1—O2^viii	42.68 (5)	O2^xiv—O3—O2ⁱⁱⁱ	149.45 (13)
O2—O1—O2^viii	86.36 (7)	Ni—O3—O2^v	82.70 (9)
O1^v—O1—O2^viii	146.77 (8)	Ni^v—O3—O2^v	42.72 (6)
O2^v—O1—O2^viii	104.32 (9)	O2^xiii—O3—O2^v	96.38 (5)
O2^vi—O1—O2^viii	90.13 (8)	O2ⁱⁱ—O3—O2^v	128.83 (9)
O3^vii—O1—O2^viii	61.69 (7)	O1ⁱ—O3—O2^v	66.62 (7)
S—O1—O3^ix	92.48 (9)	O1^vii—O3—O2^v	61.53 (7)
Ni^vi—O1—O3^ix	44.48 (5)	O2^xiv—O3—O2^v	87.96 (6)
O2—O1—O3^ix	57.76 (7)	O2ⁱⁱⁱ—O3—O2^v	121.17 (8)
O1^v—O1—O3^ix	101.39 (10)	Ni—O3—O2	42.72 (6)
O2^v—O1—O3^ix	115.60 (10)	Ni^v—O3—O2	82.70 (9)
O2^vi—O1—O3^ix	62.54 (8)	O2^xiii—O3—O2	128.83 (9)
O3^vii—O1—O3^ix	92.17 (7)	O2ⁱⁱ—O3—O2	96.38 (5)
O2^viii—O1—O3^ix	57.03 (5)	O1ⁱ—O3—O2	61.53 (7)
S—O1—O2^vii	112.55 (11)	O1^vii—O3—O2	66.62 (7)
Ni^vi—O1—O2^vii	78.42 (7)	O2^xiv—O3—O2	121.17 (8)
O2—O1—O2^vii	108.31 (8)	O2ⁱⁱⁱ—O3—O2	87.96 (6)
O1^v—O1—O2^vii	139.93 (10)	O2^v—O3—O2	47.67 (8)
O2^v—O1—O2^vii	81.19 (6)	Ni—O3—O1^xiii	122.79 (9)
O2^vi—O1—O2^vii	117.50 (9)	Ni^v—O3—O1^xiii	42.43 (4)
O3^vii—O1—O2^vii	58.91 (7)	O2^xiii—O3—O1^xiii	49.66 (5)
O2^viii—O1—O2^vii	45.78 (7)	O2ⁱⁱ—O3—O1^xiii	144.65 (6)
O3^ix—O1—O2^vii	102.59 (7)	O1ⁱ—O3—O1^xiii	80.71 (6)
S—O1—O2^x	127.54 (11)	O1^vii—O3—O1^xiii	87.83 (7)
Ni^vi—O1—O2^x	95.03 (8)	O2^xiv—O3—O1^xiii	61.25 (5)
O2—O1—O2^x	162.64 (11)	O2ⁱⁱⁱ—O3—O1^xiii	126.23 (5)
O1^v—O1—O2^x	102.58 (8)	O2^v—O3—O1^xiii	54.60 (6)
O2^v—O1—O2^x	109.36 (8)	O2—O3—O1^xiii	101.40 (9)
O2^vi—O1—O2^x	75.53 (7)	Ni—O3—O1ⁱⁱ	42.43 (4)
O3^vii—O1—O2^x	51.58 (6)	Ni^v—O3—O1ⁱⁱ	122.79 (9)
O2^viii—O1—O2^x	110.42 (8)	O2^xiii—O3—O1ⁱⁱ	144.65 (6)
O3^ix—O1—O2^x	135.00 (9)	O2ⁱⁱ—O3—O1ⁱⁱ	49.66 (5)
O2^vii—O1—O2^x	82.04 (5)	O1ⁱ—O3—O1ⁱⁱ	87.83 (7)
S—O1—O1^xi	89.75 (11)	O1^vii—O3—O1ⁱⁱ	80.71 (6)
Ni^vi—O1—O1^xi	133.20 (11)	O2^xiv—O3—O1ⁱⁱ	126.23 (5)
O2—O1—O1^xi	124.29 (11)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	61.25 (5)
O1^v—O1—O1^xi	80.91 (11)	O2^v—O3—O1ⁱⁱ	101.40 (9)
O2^v—O1—O1^xi	66.01 (8)	O2—O3—O1ⁱⁱ	54.60 (6)
O2^vi—O1—O1^xi	116.56 (11)	O1^xiii—O3—O1ⁱⁱ	155.92 (13)
O3^vii—O1—O1^xi	85.52 (7)	Ni—O3—H	106 (2)
O2^viii—O1—O1^xi	121.19 (9)	Ni^v—O3—H	107 (2)
O3^ix—O1—O1^xi	177.63 (10)	O2^xiii—O3—H	119 (2)
O2^vii—O1—O1^xi	75.79 (7)	O2ⁱⁱ—O3—H	16 (2)
O2^x—O1—O1^xi	43.35 (6)	O1ⁱ—O3—H	147 (2)
S—O2—Ni	130.46 (12)	O1^vii—O3—H	74 (2)
S—O2—O1	35.44 (7)	O2^xiv—O3—H	71 (2)
Ni—O2—O1	160.07 (10)	O2ⁱⁱⁱ—O3—H	91 (2)
S—O2—O2^v	35.53 (8)	O2^v—O3—H	136 (2)
Ni—O2—O2^v	100.61 (7)	O2—O3—H	112 (2)
O1—O2—O2^v	60.33 (7)	O1^xiii—O3—H	131 (2)
S—O2—O1^v	34.69 (6)	O1ⁱⁱ—O3—H	66 (2)
Ni—O2—O1^v	117.31 (10)	Ni—O3—H^v	107 (2)
O1—O2—O1^v	60.03 (10)	Ni^v—O3—H^v	106 (2)
O2^v—O2—O1^v	59.41 (7)	O2^xiii—O3—H^v	16 (2)
S—O2—O3^ix	106.56 (11)	O2ⁱⁱ—O3—H^v	119 (2)
Ni—O2—O3^ix	122.85 (9)	O1ⁱ—O3—H^v	74 (2)
O1—O2—O3^ix	72.58 (8)	O1^vii—O3—H^v	147 (2)
O2^v—O2—O3^ix	129.67 (10)	O2^xiv—O3—H^v	91 (2)
O1^v—O2—O3^ix	111.58 (11)	O2ⁱⁱⁱ—O3—H^v	71 (2)
S—O2—O1ⁱⁱ	160.47 (11)	O2^v—O3—H^v	112 (2)
Ni—O2—O1ⁱⁱ	47.31 (6)	O2—O3—H^v	136 (2)
O1—O2—O1ⁱⁱ	138.38 (8)	O1^xiii—O3—H^v	66 (2)
O2^v—O2—O1ⁱⁱ	127.57 (6)	O1ⁱⁱ—O3—H^v	131 (2)
O1^v—O2—O1ⁱⁱ	161.31 (11)	H—O3—H^v	107 (5)

O1^v—S—O1—Ni^vi	114.28 (19)	O2^v—S—O2—Ni	−38.93 (9)
O2—S—O1—Ni^vi	−6.6 (2)	O1^v—S—O2—O1	−121.08 (17)
O2^v—S—O1—Ni^vi	−125.77 (17)	O2^v—S—O2—O1	119.93 (10)
O1^v—S—O1—O2	120.85 (9)	O1^v—S—O2—O2^v	118.99 (10)
O2^v—S—O1—O2	−119.20 (16)	O1—S—O2—O2^v	−119.93 (10)
O2—S—O1—O1^v	−120.85 (9)	O1—S—O2—O1^v	121.08 (17)
O2^v—S—O1—O1^v	119.95 (10)	O2^v—S—O2—O1^v	−118.99 (10)
O1^v—S—O1—O2^v	−119.95 (10)	O1^v—S—O2—O3^ix	−104.16 (11)
O2—S—O1—O2^v	119.20 (16)	O1—S—O2—O3^ix	16.92 (12)
O1^v—S—O1—O2^vi	49.77 (11)	O2^v—S—O2—O3^ix	136.85 (10)
O2—S—O1—O2^vi	−71.08 (15)	O1^v—S—O2—O1ⁱⁱ	154.9 (4)
O2^v—S—O1—O2^vi	169.72 (16)	O1—S—O2—O1ⁱⁱ	−84.0 (4)
O1^v—S—O1—O2^viii	160.99 (13)	O2^v—S—O2—O1ⁱⁱ	35.9 (3)
O2—S—O1—O2^viii	40.14 (12)	O1^v—S—O2—O3ⁱⁱⁱ	13.89 (19)
O2^v—S—O1—O2^viii	−79.07 (12)	O1—S—O2—O3ⁱⁱⁱ	134.97 (15)
O1^v—S—O1—O3^ix	106.52 (8)	O2^v—S—O2—O3ⁱⁱⁱ	−105.10 (16)
O2—S—O1—O3^ix	−14.33 (11)	O1^v—S—O2—O1ⁱ	62.79 (12)
O2^v—S—O1—O3^ix	−133.54 (10)	O1—S—O2—O1ⁱ	−176.13 (9)
O1^v—S—O1—O2^vii	−148.76 (12)	O2^v—S—O2—O1ⁱ	−56.20 (6)
O2—S—O1—O2^vii	90.39 (11)	O1^v—S—O2—O3	118.99 (10)
O2^v—S—O1—O2^vii	−28.81 (13)	O1—S—O2—O3	−119.93 (10)
O1^v—S—O1—O2^x	−51.29 (9)	O2^v—S—O2—O3	0.001 (1)
O2—S—O1—O2^x	−172.14 (11)	O1^v—S—O2—O1^vii	170.29 (10)
O2^v—S—O1—O2^x	68.66 (16)	O1—S—O2—O1^vii	−68.63 (11)
O1^v—S—O1—O1^xi	−74.29 (8)	O2^v—S—O2—O1^vii	51.30 (5)
O2—S—O1—O1^xi	164.86 (9)	O1^v—S—O2—O1^xii	−47.73 (13)
O2^v—S—O1—O1^xi	45.66 (12)	O1—S—O2—O1^xii	73.35 (9)
O1^v—S—O2—Ni	80.06 (16)	O2^v—S—O2—O1^xii	−166.72 (9)
O1—S—O2—Ni	−158.85 (13)

Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) −x+1/2, y+1/2, −z+1/2; (iii) −x, −y+1, −z; (iv) x, −y+1, z−1/2; (v) −x, y, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) −x, −y, −z+1; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱ	0.84 (3)	1.87 (3)	2.667 (2)	157 (3)

Symmetry code: (ii) −x+1/2, y+1/2, −z+1/2.

(NiSO4H2O_He_45K) top

Crystal data top

H₂NiO₅S	Z = 4
M_r = 172.79	F(000) = 344
Monoclinic, C2/c	D_x = 3.358 Mg m⁻³
a = 6.7999 (8) Å	Mo Kα radiation, λ = 0.71073 Å
b = 7.6222 (6) Å	µ = 6.16 mm⁻¹
c = 7.4405 (9) Å	T = 45 K
β = 117.579 (15)°	0.34 × 0.17 × 0.12 mm
V = 341.82 (8) Å³

Data collection top

1248 measured reflections	θ_max = 29.4°, θ_min = 4.3°
422 independent reflections	h = −6→9
400 reflections with I > 2σ(I)	k = −8→10
R_int = 0.023	l = −9→8

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.020	w = 1/[σ²(F_o²) + (0.029P)² + 0.090P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.051	(Δ/σ)_max < 0.001
S = 1.11	Δρ_max = 0.56 e Å⁻³
422 reflections	Δρ_min = −0.61 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.043 (3)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ni	0.000000	0.500000	0.000000	0.00160 (19)
S	0.000000	0.15779 (9)	0.250000	0.0018 (2)
O1	0.1727 (2)	0.0479 (2)	0.4051 (2)	0.0036 (3)
O2	0.1052 (2)	0.2713 (2)	0.1554 (2)	0.0035 (3)
O3	0.000000	0.6308 (3)	0.250000	0.0035 (4)
H	0.109 (4)	0.691 (4)	0.299 (4)	0.012 (7)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni	0.0011 (3)	0.0023 (3)	0.0017 (3)	−0.00009 (11)	0.00086 (19)	−0.00006 (11)
S	0.0010 (4)	0.0022 (4)	0.0023 (4)	0.000	0.0009 (3)	0.000
O1	0.0020 (7)	0.0049 (7)	0.0039 (8)	0.0010 (6)	0.0015 (6)	0.0015 (6)
O2	0.0028 (7)	0.0043 (7)	0.0038 (7)	−0.0001 (5)	0.0018 (6)	0.0013 (5)
O3	0.0014 (10)	0.0044 (10)	0.0036 (11)	0.000	0.0003 (9)	0.000

Geometric parameters (Å, º) top

Ni—O2	2.0305 (15)	O1—O1^v	2.413 (3)
Ni—O2ⁱ	2.0305 (15)	O1—O2^v	2.426 (2)
Ni—O1ⁱⁱ	2.0320 (14)	O1—O2^vi	2.749 (2)
Ni—O1ⁱⁱⁱ	2.0320 (14)	O1—O3^vii	2.8474 (18)
Ni—O3ⁱ	2.1106 (10)	O1—O2^viii	2.9911 (19)
Ni—O3	2.1106 (10)	O1—O3^ix	3.0100 (16)
Ni—O2ⁱⁱ	3.4178 (15)	O1—O2^vii	3.210 (2)
Ni—O2ⁱⁱⁱ	3.4178 (15)	O1—O2^x	3.223 (2)
Ni—O2^iv	3.4387 (15)	O1—O1^xi	3.335 (3)
Ni—O2^v	3.4387 (15)	O2—O2^v	2.428 (3)
S—O1	1.4687 (15)	O2—O3^ix	2.6640 (17)
S—O1^v	1.4687 (15)	O2—O3ⁱ	2.8582 (16)
S—O2^v	1.4905 (15)	O2—O3	2.998 (2)
S—O2	1.4905 (15)	O3—H	0.80 (2)
O1—O2	2.402 (2)	O3—H^v	0.80 (2)

O2—Ni—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	77.81 (6)
O2—Ni—O1ⁱⁱ	94.83 (6)	S—O2—O3ⁱ	135.19 (8)
O2ⁱ—Ni—O1ⁱⁱ	85.17 (6)	Ni—O2—O3ⁱ	47.53 (5)
O2—Ni—O1ⁱⁱⁱ	85.17 (6)	O1—O2—O3ⁱ	150.00 (8)
O2ⁱ—Ni—O1ⁱⁱⁱ	94.83 (6)	O1^v—O2—O3ⁱ	101.22 (7)
O1ⁱⁱ—Ni—O1ⁱⁱⁱ	180.00 (9)	O2^v—O2—O3ⁱ	133.24 (8)
O2—Ni—O3ⁱ	87.27 (6)	O3^ix—O2—O3ⁱ	96.49 (5)
O2ⁱ—Ni—O3ⁱ	92.73 (6)	O1ⁱⁱⁱ—O2—O3ⁱ	61.00 (5)
O1ⁱⁱ—Ni—O3ⁱ	93.18 (5)	S—O2—O1ⁱⁱ	90.74 (7)
O1ⁱⁱⁱ—Ni—O3ⁱ	86.82 (5)	Ni—O2—O1ⁱⁱ	42.61 (4)
O2—Ni—O3	92.73 (6)	O1—O2—O1ⁱⁱ	126.08 (8)
O2ⁱ—Ni—O3	87.27 (6)	O1^v—O2—O1ⁱⁱ	75.57 (7)
O1ⁱⁱ—Ni—O3	86.82 (5)	O2^v—O2—O1ⁱⁱ	71.79 (6)
O1ⁱⁱⁱ—Ni—O3	93.18 (5)	O3^ix—O2—O1ⁱⁱ	158.38 (7)
O3ⁱ—Ni—O3	180.00 (10)	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.04 (6)
O2—Ni—O2ⁱⁱ	81.67 (2)	O3ⁱ—O2—O1ⁱⁱ	61.89 (5)
O2ⁱ—Ni—O2ⁱⁱ	98.33 (2)	S—O2—O3	101.58 (8)
O1ⁱⁱ—Ni—O2ⁱⁱ	43.71 (5)	Ni—O2—O3	44.69 (3)
O1ⁱⁱⁱ—Ni—O2ⁱⁱ	136.29 (5)	O1—O2—O3	116.57 (7)
O3ⁱ—Ni—O2ⁱⁱ	51.21 (3)	O1^v—O2—O3	115.78 (7)
O3—Ni—O2ⁱⁱ	128.79 (3)	O2^v—O2—O3	66.11 (3)
O2—Ni—O2ⁱⁱⁱ	98.33 (2)	O3^ix—O2—O3	128.77 (7)
O2ⁱ—Ni—O2ⁱⁱⁱ	81.67 (2)	O1ⁱⁱⁱ—O2—O3	63.00 (5)
O1ⁱⁱ—Ni—O2ⁱⁱⁱ	136.29 (5)	O3ⁱ—O2—O3	92.22 (5)
O1ⁱⁱⁱ—Ni—O2ⁱⁱⁱ	43.71 (5)	O1ⁱⁱ—O2—O3	56.78 (4)
O3ⁱ—Ni—O2ⁱⁱⁱ	128.79 (3)	S—O2—O1^vii	82.54 (7)
O3—Ni—O2ⁱⁱⁱ	51.21 (3)	Ni—O2—O1^vii	94.99 (6)
O2ⁱⁱ—Ni—O2ⁱⁱⁱ	180.0	O1—O2—O1^vii	71.64 (6)
O2—Ni—O2^iv	136.04 (6)	O1^v—O2—O1^vii	116.67 (8)
O2ⁱ—Ni—O2^iv	43.96 (6)	O2^v—O2—O1^vii	62.28 (6)
O1ⁱⁱ—Ni—O2^iv	113.85 (5)	O3^ix—O2—O1^vii	87.83 (5)
O1ⁱⁱⁱ—Ni—O2^iv	66.15 (5)	O1ⁱⁱⁱ—O2—O1^vii	78.61 (4)
O3ⁱ—Ni—O2^iv	59.84 (6)	O3ⁱ—O2—O1^vii	137.14 (7)
O3—Ni—O2^iv	120.16 (6)	O1ⁱⁱ—O2—O1^vii	107.44 (7)
O2ⁱⁱ—Ni—O2^iv	96.30 (4)	O3—O2—O1^vii	54.48 (4)
O2ⁱⁱⁱ—Ni—O2^iv	83.70 (4)	S—O2—O1^xii	93.61 (7)
O2—Ni—O2^v	43.96 (6)	Ni—O2—O1^xii	115.21 (6)
O2ⁱ—Ni—O2^v	136.04 (6)	O1—O2—O1^xii	83.38 (4)
O1ⁱⁱ—Ni—O2^v	66.15 (5)	O1^v—O2—O1^xii	70.76 (6)
O1ⁱⁱⁱ—Ni—O2^v	113.85 (5)	O2^v—O2—O1^xii	127.94 (4)
O3ⁱ—Ni—O2^v	120.16 (6)	O3^ix—O2—O1^xii	56.90 (5)
O3—Ni—O2^v	59.84 (6)	O1ⁱⁱⁱ—O2—O1^xii	104.39 (6)
O2ⁱⁱ—Ni—O2^v	83.70 (4)	O3ⁱ—O2—O1^xii	67.68 (6)
O2ⁱⁱⁱ—Ni—O2^v	96.30 (4)	O1ⁱⁱ—O2—O1^xii	110.48 (6)
O2^iv—Ni—O2^v	180.00 (4)	O3—O2—O1^xii	159.90 (6)
O1—S—O1^v	110.47 (13)	O1^vii—O2—O1^xii	141.93 (5)
O1—S—O2^v	110.13 (8)	Ni—O3—Ni^v	123.60 (10)
O1^v—S—O2^v	108.51 (8)	Ni—O3—O2^xiii	111.60 (3)
O1—S—O2	108.52 (8)	Ni^v—O3—O2^xiii	90.66 (3)
O1^v—S—O2	110.13 (8)	Ni—O3—O2ⁱⁱⁱ	90.66 (3)
O2^v—S—O2	109.07 (13)	Ni^v—O3—O2ⁱⁱⁱ	111.60 (3)
S—O1—Ni^vi	136.42 (10)	O2^xiii—O3—O2ⁱⁱⁱ	132.63 (11)
S—O1—O2	36.05 (5)	Ni—O3—O1ⁱⁱ	45.44 (4)
Ni^vi—O1—O2	100.52 (7)	Ni^v—O3—O1ⁱⁱ	104.44 (7)
S—O1—O1^v	34.76 (6)	O2^xiii—O3—O1ⁱⁱ	71.50 (4)
Ni^vi—O1—O1^v	139.20 (11)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	134.57 (5)
O2—O1—O1^v	60.51 (6)	Ni—O3—O1^vii	104.44 (7)
S—O1—O2^v	35.23 (5)	Ni^v—O3—O1^vii	45.44 (4)
Ni^vi—O1—O2^v	145.53 (9)	O2^xiii—O3—O1^vii	134.57 (5)
O2—O1—O2^v	60.38 (8)	O2ⁱⁱⁱ—O3—O1^vii	71.50 (4)
O1^v—O1—O2^v	59.52 (6)	O1ⁱⁱ—O3—O1^vii	122.82 (10)
S—O1—O2^vi	127.51 (9)	Ni—O3—O2^xiv	162.05 (7)
Ni^vi—O1—O2^vi	47.39 (4)	Ni^v—O3—O2^xiv	45.20 (3)
O2—O1—O2^vi	109.87 (6)	O2^xiii—O3—O2^xiv	84.45 (5)
O1^v—O1—O2^vi	102.05 (7)	O2ⁱⁱⁱ—O3—O2^xiv	83.51 (6)
O2^v—O1—O2^vi	161.38 (9)	O1ⁱⁱ—O3—O2^xiv	141.77 (5)
S—O1—O3^vii	171.10 (10)	O1^vii—O3—O2^xiv	57.61 (4)
Ni^vi—O1—O3^vii	47.74 (3)	Ni—O3—O2ⁱ	45.20 (3)
O2—O1—O3^vii	145.69 (7)	Ni^v—O3—O2ⁱ	162.05 (7)
O1^v—O1—O3^vii	150.51 (5)	O2^xiii—O3—O2ⁱ	83.51 (5)
O2^v—O1—O3^vii	136.02 (8)	O2ⁱⁱⁱ—O3—O2ⁱ	84.45 (5)
O2^vi—O1—O3^vii	61.39 (5)	O1ⁱⁱ—O3—O2ⁱ	57.61 (4)
S—O1—O2^viii	115.13 (9)	O1^vii—O3—O2ⁱ	141.77 (5)
Ni^vi—O1—O2^viii	42.57 (4)	O2^xiv—O3—O2ⁱ	149.73 (10)
O2—O1—O2^viii	86.32 (5)	Ni—O3—O2	42.58 (4)
O1^v—O1—O2^viii	146.79 (6)	Ni^v—O3—O2	82.66 (7)
O2^v—O1—O2^viii	104.43 (7)	O2^xiii—O3—O2	128.77 (7)
O2^vi—O1—O2^viii	89.96 (6)	O2ⁱⁱⁱ—O3—O2	96.23 (4)
O3^vii—O1—O2^viii	61.73 (5)	O1ⁱⁱ—O3—O2	61.49 (5)
S—O1—O3^ix	92.49 (7)	O1^vii—O3—O2	66.56 (6)
Ni^vi—O1—O3^ix	44.44 (4)	O2^xiv—O3—O2	121.08 (6)
O2—O1—O3^ix	57.67 (5)	O2ⁱ—O3—O2	87.78 (5)
O1^v—O1—O3^ix	101.46 (8)	Ni—O3—O2^v	82.66 (7)
O2^v—O1—O3^ix	115.62 (8)	Ni^v—O3—O2^v	42.58 (4)
O2^vi—O1—O3^ix	62.54 (6)	O2^xiii—O3—O2^v	96.23 (4)
O3^vii—O1—O3^ix	92.18 (5)	O2ⁱⁱⁱ—O3—O2^v	128.77 (7)
O2^viii—O1—O3^ix	56.88 (4)	O1ⁱⁱ—O3—O2^v	66.56 (6)
S—O1—O2^vii	112.54 (8)	O1^vii—O3—O2^v	61.49 (5)
Ni^vi—O1—O2^vii	78.47 (5)	O2^xiv—O3—O2^v	87.78 (5)
O2—O1—O2^vii	108.36 (6)	O2ⁱ—O3—O2^v	121.08 (6)
O1^v—O1—O2^vii	139.88 (8)	O2—O3—O2^v	47.78 (7)
O2^v—O1—O2^vii	81.15 (5)	Ni—O3—O1^xiii	122.70 (7)
O2^vi—O1—O2^vii	117.47 (7)	Ni^v—O3—O1^xiii	42.38 (3)
O3^vii—O1—O2^vii	58.96 (5)	O2^xiii—O3—O1^xiii	49.63 (4)
O2^viii—O1—O2^vii	45.93 (5)	O2ⁱⁱⁱ—O3—O1^xiii	144.73 (5)
O3^ix—O1—O2^vii	102.58 (5)	O1ⁱⁱ—O3—O1^xiii	80.62 (4)
S—O1—O2^x	127.46 (8)	O1^vii—O3—O1^xiii	87.82 (5)
Ni^vi—O1—O2^x	95.13 (6)	O2^xiv—O3—O1^xiii	61.22 (4)
O2—O1—O2^x	162.64 (8)	O2ⁱ—O3—O1^xiii	126.23 (4)
O1^v—O1—O2^x	102.51 (6)	O2—O3—O1^xiii	101.37 (7)
O2^v—O1—O2^x	109.24 (6)	O2^v—O3—O1^xiii	54.47 (5)
O2^vi—O1—O2^x	75.61 (6)	Ni—O3—O1ⁱⁱⁱ	42.38 (3)
O3^vii—O1—O2^x	51.60 (4)	Ni^v—O3—O1ⁱⁱⁱ	122.70 (7)
O2^viii—O1—O2^x	110.48 (6)	O2^xiii—O3—O1ⁱⁱⁱ	144.73 (5)
O3^ix—O1—O2^x	135.10 (7)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	49.63 (4)
O2^vii—O1—O2^x	82.01 (4)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	87.82 (5)
S—O1—O1^xi	89.64 (7)	O1^vii—O3—O1ⁱⁱⁱ	80.62 (4)
Ni^vi—O1—O1^xi	133.33 (9)	O2^xiv—O3—O1ⁱⁱⁱ	126.23 (4)
O2—O1—O1^xi	124.27 (8)	O2ⁱ—O3—O1ⁱⁱⁱ	61.22 (4)
O1^v—O1—O1^xi	80.81 (8)	O2—O3—O1ⁱⁱⁱ	54.47 (5)
O2^v—O1—O1^xi	65.86 (6)	O2^v—O3—O1ⁱⁱⁱ	101.37 (7)
O2^vi—O1—O1^xi	116.69 (8)	O1^xiii—O3—O1ⁱⁱⁱ	155.76 (10)
O3^vii—O1—O1^xi	85.59 (6)	Ni—O3—H	107 (2)
O2^viii—O1—O1^xi	121.30 (8)	Ni^v—O3—H	104 (2)
O3^ix—O1—O1^xi	177.69 (8)	O2^xiii—O3—H	120 (2)
O2^vii—O1—O1^xi	75.74 (6)	O2ⁱⁱⁱ—O3—H	17 (2)
O2^x—O1—O1^xi	43.38 (5)	O1ⁱⁱ—O3—H	149 (2)
S—O2—Ni	130.35 (9)	O1^vii—O3—H	72.1 (19)
S—O2—O1	35.44 (5)	O2^xiv—O3—H	69 (2)
Ni—O2—O1	160.01 (8)	O2ⁱ—O3—H	93 (2)
S—O2—O1^v	34.64 (5)	O2—O3—H	111 (2)
Ni—O2—O1^v	117.26 (7)	O2^v—O3—H	133.5 (19)
O1—O2—O1^v	59.98 (8)	O1^xiii—O3—H	130 (2)
S—O2—O2^v	35.46 (6)	O1ⁱⁱⁱ—O3—H	67 (2)
Ni—O2—O2^v	100.56 (5)	Ni—O3—H^v	104 (2)
O1—O2—O2^v	60.30 (6)	Ni^v—O3—H^v	107 (2)
O1^v—O2—O2^v	59.32 (6)	O2^xiii—O3—H^v	17 (2)
S—O2—O3^ix	106.71 (8)	O2ⁱⁱⁱ—O3—H^v	120 (2)
Ni—O2—O3^ix	122.80 (7)	O1ⁱⁱ—O3—H^v	72.1 (19)
O1—O2—O3^ix	72.70 (6)	O1^vii—O3—H^v	149 (2)
O1^v—O2—O3^ix	111.74 (8)	O2^xiv—O3—H^v	93 (2)
O2^v—O2—O3^ix	129.73 (8)	O2ⁱ—O3—H^v	69 (2)
S—O2—O1ⁱⁱⁱ	160.46 (10)	O2—O3—H^v	133.5 (19)
Ni—O2—O1ⁱⁱⁱ	47.44 (4)	O2^v—O3—H^v	111 (2)
O1—O2—O1ⁱⁱⁱ	138.36 (6)	O1^xiii—O3—H^v	67 (2)
O1^v—O2—O1ⁱⁱⁱ	161.38 (9)	O1ⁱⁱⁱ—O3—H^v	130 (2)
O2^v—O2—O1ⁱⁱⁱ	127.64 (5)	H—O3—H^v	110 (4)

O1^v—S—O1—Ni^vi	114.33 (15)	O2^v—S—O2—Ni	−38.90 (8)
O2^v—S—O1—Ni^vi	−125.82 (14)	O1^v—S—O2—O1	−121.04 (12)
O2—S—O1—Ni^vi	−6.50 (17)	O2^v—S—O2—O1	119.98 (7)
O1^v—S—O1—O2	120.82 (7)	O1—S—O2—O1^v	121.04 (12)
O2^v—S—O1—O2	−119.32 (12)	O2^v—S—O2—O1^v	−118.98 (8)
O2^v—S—O1—O1^v	119.86 (8)	O1—S—O2—O2^v	−119.98 (7)
O2—S—O1—O1^v	−120.82 (7)	O1^v—S—O2—O2^v	118.98 (8)
O1^v—S—O1—O2^v	−119.86 (8)	O1—S—O2—O3^ix	16.80 (10)
O2—S—O1—O2^v	119.32 (13)	O1^v—S—O2—O3^ix	−104.23 (9)
O1^v—S—O1—O2^vi	49.88 (8)	O2^v—S—O2—O3^ix	136.79 (8)
O2^v—S—O1—O2^vi	169.74 (12)	O1—S—O2—O1ⁱⁱⁱ	−83.9 (3)
O2—S—O1—O2^vi	−70.94 (11)	O1^v—S—O2—O1ⁱⁱⁱ	155.0 (3)
O1^v—S—O1—O2^viii	160.92 (11)	O2^v—S—O2—O1ⁱⁱⁱ	36.0 (2)
O2^v—S—O1—O2^viii	−79.22 (10)	O1—S—O2—O3ⁱ	134.81 (12)
O2—S—O1—O2^viii	40.10 (10)	O1^v—S—O2—O3ⁱ	13.78 (15)
O1^v—S—O1—O3^ix	106.62 (7)	O2^v—S—O2—O3ⁱ	−105.20 (13)
O2^v—S—O1—O3^ix	−133.52 (8)	O1—S—O2—O1ⁱⁱ	−176.15 (7)
O2—S—O1—O3^ix	−14.20 (9)	O1^v—S—O2—O1ⁱⁱ	62.81 (10)
O1^v—S—O1—O2^vii	−148.65 (9)	O2^v—S—O2—O1ⁱⁱ	−56.17 (4)
O2^v—S—O1—O2^vii	−28.80 (10)	O1—S—O2—O3	−119.98 (7)
O2—S—O1—O2^vii	90.53 (9)	O1^v—S—O2—O3	118.98 (8)
O1^v—S—O1—O2^x	−51.28 (7)	O2^v—S—O2—O3	0.0
O2^v—S—O1—O2^x	68.58 (12)	O1—S—O2—O1^vii	−68.66 (9)
O2—S—O1—O2^x	−172.10 (9)	O1^v—S—O2—O1^vii	170.30 (7)
O1^v—S—O1—O1^xi	−74.27 (6)	O2^v—S—O2—O1^vii	51.32 (4)
O2^v—S—O1—O1^xi	45.58 (9)	O1—S—O2—O1^xii	73.27 (7)
O2—S—O1—O1^xi	164.90 (8)	O1^v—S—O2—O1^xii	−47.77 (9)
O1—S—O2—Ni	−158.89 (10)	O2^v—S—O2—O1^xii	−166.75 (7)
O1^v—S—O2—Ni	80.08 (13)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x, −y+1, z−1/2; (v) −x, y, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) −x, −y, −z+1; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.80 (2)	1.91 (3)	2.6640 (17)	156 (3)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(NiSO4H2O_He_75K) top

Crystal data top

H₂NiO₅S	Z = 4
M_r = 172.79	F(000) = 344
Monoclinic, C2/c	D_x = 3.356 Mg m⁻³
a = 6.8026 (9) Å	Mo Kα radiation, λ = 0.71073 Å
b = 7.6191 (7) Å	µ = 6.16 mm⁻¹
c = 7.445 (1) Å	T = 75 K
β = 117.611 (17)°	0.34 × 0.17 × 0.12 mm
V = 341.93 (9) Å³

Data collection top

1238 measured reflections	θ_max = 29.4°, θ_min = 4.3°
424 independent reflections	h = −6→9
395 reflections with I > 2σ(I)	k = −8→10
R_int = 0.027	l = −9→8

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.021	w = 1/[σ²(F_o²) + (0.026P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.052	(Δ/σ)_max = 0.001
S = 1.12	Δρ_max = 0.44 e Å⁻³
424 reflections	Δρ_min = −0.50 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.041 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ni	0.000000	0.500000	0.000000	0.0026 (2)
S	0.000000	0.15780 (10)	0.250000	0.0028 (2)
O1	0.1724 (2)	0.0479 (2)	0.4049 (2)	0.0047 (4)
O2	0.1051 (2)	0.2709 (2)	0.1556 (2)	0.0046 (4)
O3	0.000000	0.6304 (3)	0.250000	0.0046 (5)
H	0.099 (4)	0.698 (4)	0.299 (5)	0.024 (9)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni	0.0017 (3)	0.0030 (3)	0.0031 (3)	−0.00013 (12)	0.0011 (2)	−0.00009 (13)
S	0.0018 (4)	0.0031 (4)	0.0037 (4)	0.000	0.0015 (3)	0.000
O1	0.0031 (8)	0.0049 (7)	0.0054 (8)	0.0008 (6)	0.0015 (7)	0.0012 (6)
O2	0.0037 (7)	0.0044 (8)	0.0063 (8)	0.0004 (6)	0.0028 (6)	0.0011 (6)
O3	0.0024 (11)	0.0055 (11)	0.0061 (12)	0.000	0.0022 (10)	0.000

Geometric parameters (Å, º) top

Ni—O2ⁱ	2.0324 (16)	O1—O1^iv	2.409 (3)
Ni—O2	2.0325 (16)	O1—O2^iv	2.422 (2)
Ni—O1ⁱⁱ	2.0345 (15)	O1—O2^vi	2.753 (2)
Ni—O1ⁱⁱⁱ	2.0345 (15)	O1—O3^vii	2.8471 (19)
Ni—O3	2.1097 (11)	O1—O2^viii	2.993 (2)
Ni—O3ⁱ	2.1097 (11)	O1—O3^ix	3.0124 (18)
Ni—O2ⁱⁱⁱ	3.4160 (16)	O1—O2^vii	3.212 (2)
Ni—O2ⁱⁱ	3.4160 (16)	O1—O2^x	3.223 (2)
Ni—O2^iv	3.4398 (17)	O1—O1^xi	3.334 (3)
Ni—O2^v	3.4398 (17)	O2—O2^iv	2.426 (3)
S—O1^iv	1.4670 (16)	O2—O3^ix	2.6662 (17)
S—O1	1.4670 (16)	O2—O3ⁱ	2.8623 (17)
S—O2	1.4879 (16)	O2—O3	2.995 (3)
S—O2^iv	1.4880 (16)	O3—H	0.79 (3)
O1—O2	2.399 (2)	O3—H^iv	0.79 (3)

O2ⁱ—Ni—O2	180.0	O3^ix—O2—O1ⁱⁱⁱ	77.74 (7)
O2ⁱ—Ni—O1ⁱⁱ	85.22 (6)	S—O2—O3ⁱ	135.31 (8)
O2—Ni—O1ⁱⁱ	94.78 (6)	Ni—O2—O3ⁱ	47.42 (5)
O2ⁱ—Ni—O1ⁱⁱⁱ	94.78 (6)	O1—O2—O3ⁱ	150.13 (9)
O2—Ni—O1ⁱⁱⁱ	85.22 (6)	O1^iv—O2—O3ⁱ	101.32 (7)
O1ⁱⁱ—Ni—O1ⁱⁱⁱ	180.00 (9)	O2^iv—O2—O3ⁱ	133.27 (8)
O2ⁱ—Ni—O3	87.40 (7)	O3^ix—O2—O3ⁱ	96.44 (6)
O2—Ni—O3	92.60 (7)	O1ⁱⁱⁱ—O2—O3ⁱ	60.89 (6)
O1ⁱⁱ—Ni—O3	86.77 (5)	S—O2—O1ⁱⁱ	90.74 (7)
O1ⁱⁱⁱ—Ni—O3	93.23 (5)	Ni—O2—O1ⁱⁱ	42.64 (4)
O2ⁱ—Ni—O3ⁱ	92.60 (7)	O1—O2—O1ⁱⁱ	126.08 (8)
O2—Ni—O3ⁱ	87.40 (7)	O1^iv—O2—O1ⁱⁱ	75.59 (7)
O1ⁱⁱ—Ni—O3ⁱ	93.23 (5)	O2^iv—O2—O1ⁱⁱ	71.82 (7)
O1ⁱⁱⁱ—Ni—O3ⁱ	86.77 (5)	O3^ix—O2—O1ⁱⁱ	158.31 (7)
O3—Ni—O3ⁱ	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.06 (6)
O2ⁱ—Ni—O2ⁱⁱⁱ	81.68 (3)	O3ⁱ—O2—O1ⁱⁱ	61.87 (5)
O2—Ni—O2ⁱⁱⁱ	98.32 (3)	S—O2—O3	101.51 (8)
O1ⁱⁱ—Ni—O2ⁱⁱⁱ	136.33 (5)	Ni—O2—O3	44.72 (3)
O1ⁱⁱⁱ—Ni—O2ⁱⁱⁱ	43.67 (5)	O1—O2—O3	116.53 (7)
O3—Ni—O2ⁱⁱⁱ	51.30 (4)	O1^iv—O2—O3	115.78 (7)
O3ⁱ—Ni—O2ⁱⁱⁱ	128.70 (4)	O2^iv—O2—O3	66.11 (4)
O2ⁱ—Ni—O2ⁱⁱ	98.32 (3)	O3^ix—O2—O3	128.78 (7)
O2—Ni—O2ⁱⁱ	81.68 (3)	O1ⁱⁱⁱ—O2—O3	63.04 (5)
O1ⁱⁱ—Ni—O2ⁱⁱ	43.67 (5)	O3ⁱ—O2—O3	92.14 (5)
O1ⁱⁱⁱ—Ni—O2ⁱⁱ	136.33 (5)	O1ⁱⁱ—O2—O3	56.78 (4)
O3—Ni—O2ⁱⁱ	128.70 (4)	S—O2—O1^vii	82.55 (7)
O3ⁱ—Ni—O2ⁱⁱ	51.30 (4)	Ni—O2—O1^vii	94.98 (6)
O2ⁱⁱⁱ—Ni—O2ⁱⁱ	180.0	O1—O2—O1^vii	71.65 (7)
O2ⁱ—Ni—O2^iv	136.12 (6)	O1^iv—O2—O1^vii	116.72 (9)
O2—Ni—O2^iv	43.88 (6)	O2^iv—O2—O1^vii	62.32 (7)
O1ⁱⁱ—Ni—O2^iv	66.16 (6)	O3^ix—O2—O1^vii	87.84 (5)
O1ⁱⁱⁱ—Ni—O2^iv	113.84 (6)	O1ⁱⁱⁱ—O2—O1^vii	78.57 (4)
O3—Ni—O2^iv	59.75 (6)	O3ⁱ—O2—O1^vii	136.99 (7)
O3ⁱ—Ni—O2^iv	120.25 (6)	O1ⁱⁱ—O2—O1^vii	107.46 (7)
O2ⁱⁱⁱ—Ni—O2^iv	96.30 (4)	O3—O2—O1^vii	54.47 (4)
O2ⁱⁱ—Ni—O2^iv	83.70 (4)	S—O2—O1^xii	93.74 (8)
O2ⁱ—Ni—O2^v	43.88 (6)	Ni—O2—O1^xii	115.10 (7)
O2—Ni—O2^v	136.12 (6)	O1—O2—O1^xii	83.50 (5)
O1ⁱⁱ—Ni—O2^v	113.84 (6)	O1^iv—O2—O1^xii	70.80 (7)
O1ⁱⁱⁱ—Ni—O2^v	66.16 (6)	O2^iv—O2—O1^xii	128.01 (5)
O3—Ni—O2^v	120.25 (6)	O3^ix—O2—O1^xii	56.89 (5)
O3ⁱ—Ni—O2^v	59.75 (6)	O1ⁱⁱⁱ—O2—O1^xii	104.28 (6)
O2ⁱⁱⁱ—Ni—O2^v	83.70 (4)	O3ⁱ—O2—O1^xii	67.68 (6)
O2ⁱⁱ—Ni—O2^v	96.30 (4)	O1ⁱⁱ—O2—O1^xii	110.43 (7)
O2^iv—Ni—O2^v	180.00 (4)	O3—O2—O1^xii	159.82 (6)
O1^iv—S—O1	110.41 (13)	O1^vii—O2—O1^xii	141.96 (6)
O1^iv—S—O2	110.06 (9)	Ni—O3—Ni^iv	123.83 (11)
O1—S—O2	108.55 (9)	Ni—O3—O2^xiii	111.62 (4)
O1^iv—S—O2^iv	108.55 (9)	Ni^iv—O3—O2^xiii	90.56 (4)
O1—S—O2^iv	110.06 (9)	Ni—O3—O2ⁱⁱⁱ	90.56 (4)
O2—S—O2^iv	109.20 (13)	Ni^iv—O3—O2ⁱⁱⁱ	111.62 (4)
S—O1—Ni^vi	136.35 (11)	O2^xiii—O3—O2ⁱⁱⁱ	132.63 (11)
S—O1—O2	36.02 (6)	Ni—O3—O1ⁱⁱ	45.52 (4)
Ni^vi—O1—O2	100.48 (7)	Ni^iv—O3—O1ⁱⁱ	104.56 (8)
S—O1—O1^iv	34.80 (7)	O2^xiii—O3—O1ⁱⁱ	71.45 (5)
Ni^vi—O1—O1^iv	139.15 (12)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	134.54 (5)
O2—O1—O1^iv	60.48 (6)	Ni—O3—O1^vii	104.56 (8)
S—O1—O2^iv	35.25 (6)	Ni^iv—O3—O1^vii	45.52 (4)
Ni^vi—O1—O2^iv	145.52 (9)	O2^xiii—O3—O1^vii	134.54 (5)
O2—O1—O2^iv	60.42 (8)	O2ⁱⁱⁱ—O3—O1^vii	71.45 (5)
O1^iv—O1—O2^iv	59.55 (6)	O1ⁱⁱ—O3—O1^vii	123.01 (10)
S—O1—O2^vi	127.49 (10)	Ni—O3—O2^xiv	162.23 (8)
Ni^vi—O1—O2^vi	47.36 (5)	Ni^iv—O3—O2^xiv	45.18 (3)
O2—O1—O2^vi	109.79 (7)	O2^xiii—O3—O2^xiv	84.32 (5)
O1^iv—O1—O2^vi	102.04 (7)	O2ⁱⁱⁱ—O3—O2^xiv	83.56 (6)
O2^iv—O1—O2^vi	161.39 (10)	O1ⁱⁱ—O3—O2^xiv	141.78 (6)
S—O1—O3^vii	171.05 (11)	O1^vii—O3—O2^xiv	57.66 (5)
Ni^vi—O1—O3^vii	47.72 (3)	Ni—O3—O2ⁱ	45.18 (3)
O2—O1—O3^vii	145.60 (7)	Ni^iv—O3—O2ⁱ	162.23 (8)
O1^iv—O1—O3^vii	150.62 (6)	O2^xiii—O3—O2ⁱ	83.56 (6)
O2^iv—O1—O3^vii	135.99 (9)	O2ⁱⁱⁱ—O3—O2ⁱ	84.32 (5)
O2^vi—O1—O3^vii	61.44 (5)	O1ⁱⁱ—O3—O2ⁱ	57.66 (5)
S—O1—O2^viii	115.07 (9)	O1^vii—O3—O2ⁱ	141.78 (6)
Ni^vi—O1—O2^viii	42.58 (4)	O2^xiv—O3—O2ⁱ	149.53 (11)
O2—O1—O2^viii	86.31 (5)	Ni—O3—O2	42.68 (5)
O1^iv—O1—O2^viii	146.76 (7)	Ni^iv—O3—O2	82.77 (8)
O2^iv—O1—O2^viii	104.41 (7)	O2^xiii—O3—O2	128.78 (7)
O2^vi—O1—O2^viii	89.94 (6)	O2ⁱⁱⁱ—O3—O2	96.22 (4)
O3^vii—O1—O2^viii	61.64 (6)	O1ⁱⁱ—O3—O2	61.58 (6)
S—O1—O3^ix	92.50 (8)	O1^vii—O3—O2	66.64 (6)
Ni^vi—O1—O3^ix	44.37 (4)	O2^xiv—O3—O2	121.19 (7)
O2—O1—O3^ix	57.71 (6)	O2ⁱ—O3—O2	87.86 (5)
O1^iv—O1—O3^ix	101.43 (9)	Ni—O3—O2^iv	82.77 (8)
O2^iv—O1—O3^ix	115.70 (8)	Ni^iv—O3—O2^iv	42.68 (5)
O2^vi—O1—O3^ix	62.40 (6)	O2^xiii—O3—O2^iv	96.22 (4)
O3^vii—O1—O3^ix	92.08 (5)	O2ⁱⁱⁱ—O3—O2^iv	128.78 (7)
O2^viii—O1—O3^ix	56.92 (4)	O1ⁱⁱ—O3—O2^iv	66.64 (6)
S—O1—O2^vii	112.54 (9)	O1^vii—O3—O2^iv	61.58 (6)
Ni^vi—O1—O2^vii	78.43 (6)	O2^xiv—O3—O2^iv	87.86 (5)
O2—O1—O2^vii	108.35 (7)	O2ⁱ—O3—O2^iv	121.19 (7)
O1^iv—O1—O2^vii	139.95 (8)	O2—O3—O2^iv	47.78 (7)
O2^iv—O1—O2^vii	81.17 (6)	Ni—O3—O1^xiii	122.83 (7)
O2^vi—O1—O2^vii	117.43 (7)	Ni^iv—O3—O1^xiii	42.40 (3)
O3^vii—O1—O2^vii	58.89 (6)	O2^xiii—O3—O1^xiii	49.52 (5)
O2^viii—O1—O2^vii	45.86 (6)	O2ⁱⁱⁱ—O3—O1^xiii	144.76 (5)
O3^ix—O1—O2^vii	102.56 (6)	O1ⁱⁱ—O3—O1^xiii	80.64 (4)
S—O1—O2^x	127.52 (8)	O1^vii—O3—O1^xiii	87.92 (5)
Ni^vi—O1—O2^x	95.16 (6)	O2^xiv—O3—O1^xiii	61.20 (4)
O2—O1—O2^x	162.67 (8)	O2ⁱ—O3—O1^xiii	126.25 (4)
O1^iv—O1—O2^x	102.58 (6)	O2—O3—O1^xiii	101.46 (7)
O2^iv—O1—O2^x	109.20 (7)	O2^iv—O3—O1^xiii	54.56 (5)
O2^vi—O1—O2^x	75.72 (6)	Ni—O3—O1ⁱⁱⁱ	42.40 (3)
O3^vii—O1—O2^x	51.66 (5)	Ni^iv—O3—O1ⁱⁱⁱ	122.83 (7)
O2^viii—O1—O2^x	110.43 (7)	O2^xiii—O3—O1ⁱⁱⁱ	144.76 (5)
O3^ix—O1—O2^x	135.05 (7)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	49.52 (5)
O2^vii—O1—O2^x	81.97 (4)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	87.92 (5)
S—O1—O1^xi	89.75 (8)	O1^vii—O3—O1ⁱⁱⁱ	80.64 (4)
Ni^vi—O1—O1^xi	133.28 (9)	O2^xiv—O3—O1ⁱⁱⁱ	126.25 (4)
O2—O1—O1^xi	124.35 (8)	O2ⁱ—O3—O1ⁱⁱⁱ	61.20 (4)
O1^iv—O1—O1^xi	80.94 (8)	O2—O3—O1ⁱⁱⁱ	54.56 (5)
O2^iv—O1—O1^xi	65.90 (7)	O2^iv—O3—O1ⁱⁱⁱ	101.46 (7)
O2^vi—O1—O1^xi	116.74 (9)	O1^xiii—O3—O1ⁱⁱⁱ	155.93 (10)
O3^vii—O1—O1^xi	85.57 (6)	Ni—O3—H	111 (3)
O2^viii—O1—O1^xi	121.21 (8)	Ni^iv—O3—H	105 (2)
O3^ix—O1—O1^xi	177.58 (8)	O2^xiii—O3—H	114 (2)
O2^vii—O1—O1^xi	75.73 (7)	O2ⁱⁱⁱ—O3—H	22 (2)
O2^x—O1—O1^xi	43.31 (5)	O1ⁱⁱ—O3—H	150 (3)
S—O2—Ni	130.37 (9)	O1^vii—O3—H	76 (2)
S—O2—O1	35.43 (5)	O2^xiv—O3—H	67 (3)
Ni—O2—O1	160.01 (9)	O2ⁱ—O3—H	93 (2)
S—O2—O1^iv	34.68 (5)	O2—O3—H	117 (2)
Ni—O2—O1^iv	117.30 (7)	O2^iv—O3—H	137 (2)
O1—O2—O1^iv	59.98 (8)	O1^xiii—O3—H	126 (3)
S—O2—O2^iv	35.40 (7)	O1ⁱⁱⁱ—O3—H	72 (2)
Ni—O2—O2^iv	100.62 (5)	Ni—O3—H^iv	105 (2)
O1—O2—O2^iv	60.25 (6)	Ni^iv—O3—H^iv	111 (3)
O1^iv—O2—O2^iv	59.33 (6)	O2^xiii—O3—H^iv	22 (2)
S—O2—O3^ix	106.78 (9)	O2ⁱⁱⁱ—O3—H^iv	114 (2)
Ni—O2—O3^ix	122.71 (8)	O1ⁱⁱ—O3—H^iv	76 (2)
O1—O2—O3^ix	72.77 (6)	O1^vii—O3—H^iv	150 (3)
O1^iv—O2—O3^ix	111.74 (9)	O2^xiv—O3—H^iv	93 (2)
O2^iv—O2—O3^ix	129.76 (9)	O2ⁱ—O3—H^iv	67 (3)
S—O2—O1ⁱⁱⁱ	160.43 (10)	O2—O3—H^iv	137 (2)
Ni—O2—O1ⁱⁱⁱ	47.42 (5)	O2^iv—O3—H^iv	117 (2)
O1—O2—O1ⁱⁱⁱ	138.35 (6)	O1^xiii—O3—H^iv	72 (2)
O1^iv—O2—O1ⁱⁱⁱ	161.39 (10)	O1ⁱⁱⁱ—O3—H^iv	126 (3)
O2^iv—O2—O1ⁱⁱⁱ	127.68 (6)	H—O3—H^iv	99 (4)

O1^iv—S—O1—Ni^vi	114.32 (16)	O2^iv—S—O2—Ni	−38.87 (8)
O2—S—O1—Ni^vi	−6.41 (17)	O1^iv—S—O2—O1	−120.94 (13)
O2^iv—S—O1—Ni^vi	−125.87 (14)	O2^iv—S—O2—O1	120.00 (8)
O1^iv—S—O1—O2	120.73 (8)	O1—S—O2—O1^iv	120.94 (13)
O2^iv—S—O1—O2	−119.46 (13)	O2^iv—S—O2—O1^iv	−119.06 (8)
O2—S—O1—O1^iv	−120.73 (8)	O1^iv—S—O2—O2^iv	119.06 (8)
O2^iv—S—O1—O1^iv	119.81 (8)	O1—S—O2—O2^iv	−120.00 (8)
O1^iv—S—O1—O2^iv	−119.81 (8)	O1^iv—S—O2—O3^ix	−104.14 (9)
O2—S—O1—O2^iv	119.46 (13)	O1—S—O2—O3^ix	16.80 (11)
O1^iv—S—O1—O2^vi	49.96 (8)	O2^iv—S—O2—O3^ix	136.80 (9)
O2—S—O1—O2^vi	−70.77 (12)	O1^iv—S—O2—O1ⁱⁱⁱ	155.1 (3)
O2^iv—S—O1—O2^vi	169.77 (13)	O1—S—O2—O1ⁱⁱⁱ	−83.9 (3)
O1^iv—S—O1—O2^viii	160.90 (12)	O2^iv—S—O2—O1ⁱⁱⁱ	36.1 (2)
O2—S—O1—O2^viii	40.17 (11)	O1^iv—S—O2—O3ⁱ	13.99 (15)
O2^iv—S—O1—O2^viii	−79.29 (11)	O1—S—O2—O3ⁱ	134.93 (13)
O1^iv—S—O1—O3^ix	106.53 (7)	O2^iv—S—O2—O3ⁱ	−105.07 (13)
O2—S—O1—O3^ix	−14.19 (9)	O1^iv—S—O2—O1ⁱⁱ	62.88 (10)
O2^iv—S—O1—O3^ix	−133.65 (8)	O1—S—O2—O1ⁱⁱ	−176.18 (8)
O1^iv—S—O1—O2^vii	−148.77 (10)	O2^iv—S—O2—O1ⁱⁱ	−56.18 (5)
O2—S—O1—O2^vii	90.51 (10)	O1^iv—S—O2—O3	119.06 (8)
O2^iv—S—O1—O2^vii	−28.95 (10)	O1—S—O2—O3	−120.00 (8)
O1^iv—S—O1—O2^x	−51.41 (7)	O2^iv—S—O2—O3	0.000 (1)
O2—S—O1—O2^x	−172.13 (10)	O1^iv—S—O2—O1^vii	170.40 (8)
O2^iv—S—O1—O2^x	68.41 (13)	O1—S—O2—O1^vii	−68.66 (9)
O1^iv—S—O1—O1^xi	−74.35 (6)	O2^iv—S—O2—O1^vii	51.34 (4)
O2—S—O1—O1^xi	164.92 (8)	O1^iv—S—O2—O1^xii	−47.65 (9)
O2^iv—S—O1—O1^xi	45.46 (9)	O1—S—O2—O1^xii	73.29 (8)
O1^iv—S—O2—Ni	80.19 (14)	O2^iv—S—O2—O1^xii	−166.71 (7)
O1—S—O2—Ni	−158.87 (11)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x, y, −z+1/2; (v) x, −y+1, z−1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) −x, −y, −z+1; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.79 (3)	1.96 (3)	2.6662 (17)	149 (3)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(NiSO4H2O_N2_113K) top

Crystal data top

H₂NiO₅S	V = 341.66 (9) Å³
M_r = 172.79	Z = 4
Monoclinic, C2/c	F(000) = 344
a = 6.8037 (10) Å	D_x = 3.359 Mg m⁻³
b = 7.6178 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.4371 (10) Å	µ = 6.17 mm⁻¹
β = 117.58 (1)°	T = 113 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.024
T_min = 0.662, T_max = 0.748	θ_max = 40.0°, θ_min = 4.3°
10699 measured reflections	h = −12→12
1061 independent reflections	k = −13→13
1034 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.016	w = 1/[σ²(F_o²) + (0.021P)² + 0.530P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.042	(Δ/σ)_max < 0.001
S = 1.12	Δρ_max = 0.83 e Å⁻³
1061 reflections	Δρ_min = −0.67 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0186 (13)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ni	0.000000	0.500000	0.000000	0.00292 (5)
S	0.000000	0.15763 (4)	0.250000	0.00284 (5)
O1	0.17257 (10)	0.04772 (9)	0.40473 (9)	0.00604 (10)
O2	0.10507 (10)	0.27108 (8)	0.15552 (9)	0.00506 (9)
O3	0.000000	0.63055 (12)	0.250000	0.00491 (12)
H	0.109 (3)	0.695 (3)	0.294 (3)	0.020 (5)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni	0.00272 (6)	0.00320 (7)	0.00283 (6)	−0.00010 (4)	0.00127 (5)	0.00010 (3)
S	0.00228 (9)	0.00297 (10)	0.00321 (9)	0.000	0.00121 (7)	0.000
O1	0.0039 (2)	0.0070 (2)	0.0067 (2)	0.00183 (17)	0.00202 (17)	0.00315 (17)
O2	0.0051 (2)	0.0047 (2)	0.0067 (2)	0.00031 (16)	0.00378 (17)	0.00181 (16)
O3	0.0042 (3)	0.0056 (3)	0.0050 (3)	0.000	0.0022 (2)	0.000

Geometric parameters (Å, º) top

Ni—O2	2.0309 (6)	O1—O1^v	2.4097 (13)
Ni—O2ⁱ	2.0309 (6)	O1—O2^v	2.4249 (9)
Ni—O1ⁱⁱ	2.0336 (7)	O1—O2^vi	2.7493 (9)
Ni—O1ⁱⁱⁱ	2.0336 (7)	O1—O3^vii	2.8467 (8)
Ni—O3ⁱ	2.1085 (5)	O1—O2^viii	2.9935 (10)
Ni—O3	2.1085 (5)	O1—O3^ix	3.0098 (7)
Ni—O2ⁱⁱ	3.4166 (7)	O1—O2^vii	3.2108 (10)
Ni—O2ⁱⁱⁱ	3.4166 (7)	O1—O2^x	3.2219 (9)
Ni—O2^iv	3.4368 (7)	O1—O1^xi	3.3365 (13)
Ni—O2^v	3.4368 (7)	O2—O2^v	2.4247 (12)
S—O1^v	1.4672 (7)	O2—O3^ix	2.6667 (8)
S—O1	1.4672 (7)	O2—O3ⁱ	2.8587 (8)
S—O2^v	1.4888 (6)	O2—O3	2.9948 (11)
S—O2	1.4888 (6)	O3—H	0.82 (2)
O1—O2	2.3985 (9)	O3—H^v	0.82 (2)

O2—Ni—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	77.72 (3)
O2—Ni—O1ⁱⁱ	94.87 (3)	S—O2—O3ⁱ	135.23 (4)
O2ⁱ—Ni—O1ⁱⁱ	85.13 (3)	Ni—O2—O3ⁱ	47.46 (2)
O2—Ni—O1ⁱⁱⁱ	85.13 (3)	O1—O2—O3ⁱ	150.01 (4)
O2ⁱ—Ni—O1ⁱⁱⁱ	94.87 (3)	O2^v—O2—O3ⁱ	133.23 (4)
O1ⁱⁱ—Ni—O1ⁱⁱⁱ	180.0	O1^v—O2—O3ⁱ	101.31 (3)
O2—Ni—O3ⁱ	87.33 (3)	O3^ix—O2—O3ⁱ	96.46 (2)
O2ⁱ—Ni—O3ⁱ	92.67 (3)	O1ⁱⁱⁱ—O2—O3ⁱ	60.97 (2)
O1ⁱⁱ—Ni—O3ⁱ	93.19 (2)	S—O2—O1ⁱⁱ	90.77 (3)
O1ⁱⁱⁱ—Ni—O3ⁱ	86.81 (2)	Ni—O2—O1ⁱⁱ	42.600 (17)
O2—Ni—O3	92.67 (3)	O1—O2—O1ⁱⁱ	126.15 (4)
O2ⁱ—Ni—O3	87.33 (3)	O2^v—O2—O1ⁱⁱ	71.81 (3)
O1ⁱⁱ—Ni—O3	86.81 (2)	O1^v—O2—O1ⁱⁱ	75.61 (3)
O1ⁱⁱⁱ—Ni—O3	93.19 (2)	O3^ix—O2—O1ⁱⁱ	158.30 (3)
O3ⁱ—Ni—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.08 (3)
O2—Ni—O2ⁱⁱ	81.681 (14)	O3ⁱ—O2—O1ⁱⁱ	61.85 (2)
O2ⁱ—Ni—O2ⁱⁱ	98.320 (15)	S—O2—O3	101.60 (3)
O1ⁱⁱ—Ni—O2ⁱⁱ	43.64 (2)	Ni—O2—O3	44.693 (16)
O1ⁱⁱⁱ—Ni—O2ⁱⁱ	136.36 (2)	O1—O2—O3	116.65 (3)
O3ⁱ—Ni—O2ⁱⁱ	51.304 (16)	O2^v—O2—O3	66.120 (14)
O3—Ni—O2ⁱⁱ	128.696 (16)	O1^v—O2—O3	115.77 (3)
O2—Ni—O2ⁱⁱⁱ	98.320 (14)	O3^ix—O2—O3	128.76 (3)
O2ⁱ—Ni—O2ⁱⁱⁱ	81.680 (15)	O1ⁱⁱⁱ—O2—O3	63.03 (2)
O1ⁱⁱ—Ni—O2ⁱⁱⁱ	136.36 (2)	O3ⁱ—O2—O3	92.15 (2)
O1ⁱⁱⁱ—Ni—O2ⁱⁱⁱ	43.64 (2)	O1ⁱⁱ—O2—O3	56.769 (17)
O3ⁱ—Ni—O2ⁱⁱⁱ	128.696 (16)	S—O2—O1^vii	82.62 (3)
O3—Ni—O2ⁱⁱⁱ	51.304 (16)	Ni—O2—O1^vii	94.97 (3)
O2ⁱⁱ—Ni—O2ⁱⁱⁱ	180.00 (2)	O1—O2—O1^vii	71.73 (3)
O2—Ni—O2^iv	136.09 (2)	O2^v—O2—O1^vii	62.34 (3)
O2ⁱ—Ni—O2^iv	43.91 (2)	O1^v—O2—O1^vii	116.70 (3)
O1ⁱⁱ—Ni—O2^iv	113.79 (2)	O3^ix—O2—O1^vii	87.83 (2)
O1ⁱⁱⁱ—Ni—O2^iv	66.21 (2)	O1ⁱⁱⁱ—O2—O1^vii	78.53 (2)
O3ⁱ—Ni—O2^iv	59.81 (3)	O3ⁱ—O2—O1^vii	137.03 (3)
O3—Ni—O2^iv	120.19 (3)	O1ⁱⁱ—O2—O1^vii	107.46 (3)
O2ⁱⁱ—Ni—O2^iv	96.345 (19)	O3—O2—O1^vii	54.477 (17)
O2ⁱⁱⁱ—Ni—O2^iv	83.655 (18)	S—O2—O1^xii	93.67 (3)
O2—Ni—O2^v	43.91 (2)	Ni—O2—O1^xii	115.12 (3)
O2ⁱ—Ni—O2^v	136.09 (2)	O1—O2—O1^xii	83.40 (2)
O1ⁱⁱ—Ni—O2^v	66.21 (2)	O2^v—O2—O1^xii	128.01 (2)
O1ⁱⁱⁱ—Ni—O2^v	113.79 (2)	O1^v—O2—O1^xii	70.84 (3)
O3ⁱ—Ni—O2^v	120.19 (3)	O3^ix—O2—O1^xii	56.88 (2)
O3—Ni—O2^v	59.81 (3)	O1ⁱⁱⁱ—O2—O1^xii	104.29 (3)
O2ⁱⁱ—Ni—O2^v	83.655 (19)	O3ⁱ—O2—O1^xii	67.66 (3)
O2ⁱⁱⁱ—Ni—O2^v	96.345 (18)	O1ⁱⁱ—O2—O1^xii	110.45 (3)
O2^iv—Ni—O2^v	180.000 (12)	O3—O2—O1^xii	159.81 (3)
O1^v—S—O1	110.41 (6)	O1^vii—O2—O1^xii	141.95 (2)
O1^v—S—O2^v	108.46 (4)	Ni—O3—Ni^v	123.72 (4)
O1—S—O2^v	110.23 (4)	Ni—O3—O2^xiii	111.614 (17)
O1^v—S—O2	110.23 (4)	Ni^v—O3—O2^xiii	90.591 (16)
O1—S—O2	108.46 (4)	Ni—O3—O2ⁱⁱⁱ	90.591 (16)
O2^v—S—O2	109.04 (5)	Ni^v—O3—O2ⁱⁱⁱ	111.614 (17)
S—O1—Ni^vi	136.47 (4)	O2^xiii—O3—O2ⁱⁱⁱ	132.67 (5)
S—O1—O2	36.07 (2)	Ni—O3—O1ⁱⁱ	45.499 (17)
Ni^vi—O1—O2	100.54 (3)	Ni^v—O3—O1ⁱⁱ	104.53 (3)
S—O1—O1^v	34.80 (3)	O2^xiii—O3—O1ⁱⁱ	71.43 (2)
Ni^vi—O1—O1^v	139.35 (4)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	134.54 (2)
O2—O1—O1^v	60.57 (3)	Ni—O3—O1^vii	104.53 (3)
S—O1—O2^v	35.18 (2)	Ni^v—O3—O1^vii	45.499 (17)
Ni^vi—O1—O2^v	145.47 (4)	O2^xiii—O3—O1^vii	134.54 (2)
O2—O1—O2^v	60.36 (3)	O2ⁱⁱⁱ—O3—O1^vii	71.43 (2)
O1^v—O1—O2^v	59.48 (2)	O1ⁱⁱ—O3—O1^vii	123.01 (4)
S—O1—O2^vi	127.63 (4)	Ni—O3—O2^xiv	162.15 (3)
Ni^vi—O1—O2^vi	47.393 (19)	Ni^v—O3—O2^xiv	45.207 (15)
O2—O1—O2^vi	109.93 (3)	O2^xiii—O3—O2^xiv	84.38 (2)
O1^v—O1—O2^vi	102.17 (3)	O2ⁱⁱⁱ—O3—O2^xiv	83.54 (2)
O2^v—O1—O2^vi	161.46 (4)	O1ⁱⁱ—O3—O2^xiv	141.79 (2)
S—O1—O3^vii	170.96 (4)	O1^vii—O3—O2^xiv	57.62 (2)
Ni^vi—O1—O3^vii	47.692 (15)	Ni—O3—O2ⁱ	45.207 (15)
O2—O1—O3^vii	145.62 (3)	Ni^v—O3—O2ⁱ	162.15 (3)
O1^v—O1—O3^vii	150.59 (2)	O2^xiii—O3—O2ⁱ	83.54 (2)
O2^v—O1—O3^vii	135.95 (3)	O2ⁱⁱⁱ—O3—O2ⁱ	84.38 (2)
O2^vi—O1—O3^vii	61.41 (2)	O1ⁱⁱ—O3—O2ⁱ	57.62 (2)
S—O1—O2^viii	115.11 (4)	O1^vii—O3—O2ⁱ	141.79 (2)
Ni^vi—O1—O2^viii	42.530 (19)	O2^xiv—O3—O2ⁱ	149.60 (4)
O2—O1—O2^viii	86.31 (2)	Ni—O3—O2	42.641 (19)
O1^v—O1—O2^viii	146.85 (3)	Ni^v—O3—O2	82.71 (3)
O2^v—O1—O2^viii	104.39 (3)	O2^xiii—O3—O2	128.76 (3)
O2^vi—O1—O2^viii	89.92 (3)	O2ⁱⁱⁱ—O3—O2	96.202 (18)
O3^vii—O1—O2^viii	61.64 (2)	O1ⁱⁱ—O3—O2	61.59 (2)
S—O1—O3^ix	92.62 (3)	O1^vii—O3—O2	66.63 (3)
Ni^vi—O1—O3^ix	44.385 (17)	O2^xiv—O3—O2	121.13 (3)
O2—O1—O3^ix	57.77 (2)	O2ⁱ—O3—O2	87.85 (2)
O1^v—O1—O3^ix	101.62 (4)	Ni—O3—O2^v	82.71 (3)
O2^v—O1—O3^ix	115.68 (3)	Ni^v—O3—O2^v	42.641 (19)
O2^vi—O1—O3^ix	62.47 (3)	O2^xiii—O3—O2^v	96.202 (17)
O3^vii—O1—O3^ix	92.08 (2)	O2ⁱⁱⁱ—O3—O2^v	128.76 (3)
O2^viii—O1—O3^ix	56.87 (2)	O1ⁱⁱ—O3—O2^v	66.63 (3)
S—O1—O2^vii	112.47 (4)	O1^vii—O3—O2^v	61.59 (2)
Ni^vi—O1—O2^vii	78.37 (2)	O2^xiv—O3—O2^v	87.85 (2)
O2—O1—O2^vii	108.27 (3)	O2ⁱ—O3—O2^v	121.13 (3)
O1^v—O1—O2^vii	139.83 (3)	O2—O3—O2^v	47.76 (3)
O2^v—O1—O2^vii	81.14 (2)	Ni—O3—O1^xiii	122.71 (3)
O2^vi—O1—O2^vii	117.40 (3)	Ni^v—O3—O1^xiii	42.424 (14)
O3^vii—O1—O2^vii	58.89 (2)	O2^xiii—O3—O1^xiii	49.536 (19)
O2^viii—O1—O2^vii	45.85 (2)	O2ⁱⁱⁱ—O3—O1^xiii	144.81 (2)
O3^ix—O1—O2^vii	102.49 (2)	O1ⁱⁱ—O3—O1^xiii	80.57 (2)
S—O1—O2^x	127.40 (4)	O1^vii—O3—O1^xiii	87.92 (2)
Ni^vi—O1—O2^x	95.18 (3)	O2^xiv—O3—O1^xiii	61.28 (2)
O2—O1—O2^x	162.63 (4)	O2ⁱ—O3—O1^xiii	126.19 (2)
O1^v—O1—O2^x	102.46 (3)	O2—O3—O1^xiii	101.38 (3)
O2^v—O1—O2^x	109.16 (3)	O2^v—O3—O1^xiii	54.50 (2)
O2^vi—O1—O2^x	75.71 (3)	Ni—O3—O1ⁱⁱⁱ	42.424 (13)
O3^vii—O1—O2^x	51.68 (2)	Ni^v—O3—O1ⁱⁱⁱ	122.71 (3)
O2^viii—O1—O2^x	110.45 (3)	O2^xiii—O3—O1ⁱⁱⁱ	144.81 (2)
O3^ix—O1—O2^x	135.11 (3)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	49.536 (19)
O2^vii—O1—O2^x	81.988 (19)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	87.92 (2)
S—O1—O1^xi	89.57 (3)	O1^vii—O3—O1ⁱⁱⁱ	80.57 (2)
Ni^vi—O1—O1^xi	133.31 (4)	O2^xiv—O3—O1ⁱⁱⁱ	126.192 (19)
O2—O1—O1^xi	124.21 (4)	O2ⁱ—O3—O1ⁱⁱⁱ	61.28 (2)
O1^v—O1—O1^xi	80.76 (3)	O2—O3—O1ⁱⁱⁱ	54.50 (2)
O2^v—O1—O1^xi	65.81 (3)	O2^v—O3—O1ⁱⁱⁱ	101.38 (3)
O2^vi—O1—O1^xi	116.79 (4)	O1^xiii—O3—O1ⁱⁱⁱ	155.80 (4)
O3^vii—O1—O1^xi	85.62 (3)	Ni—O3—H	105.3 (15)
O2^viii—O1—O1^xi	121.19 (3)	Ni^v—O3—H	107.3 (15)
O3^ix—O1—O1^xi	177.60 (3)	O2^xiii—O3—H	118.9 (15)
O2^vii—O1—O1^xi	75.73 (3)	O2ⁱⁱⁱ—O3—H	16.1 (15)
O2^x—O1—O1^xi	43.355 (19)	O1ⁱⁱ—O3—H	146.2 (15)
S—O2—Ni	130.38 (4)	O1^vii—O3—H	74.7 (15)
S—O2—O1	35.47 (2)	O2^xiv—O3—H	71.6 (15)
Ni—O2—O1	160.09 (4)	O2ⁱ—O3—H	90.3 (15)
S—O2—O2^v	35.48 (3)	O2—O3—H	111.5 (15)
Ni—O2—O2^v	100.58 (2)	O2^v—O3—H	136.1 (15)
O1—O2—O2^v	60.36 (3)	O1^xiii—O3—H	131.8 (15)
S—O2—O1^v	34.59 (2)	O1ⁱⁱⁱ—O3—H	65.4 (15)
Ni—O2—O1^v	117.30 (3)	Ni—O3—H^v	107.3 (15)
O1—O2—O1^v	59.94 (3)	Ni^v—O3—H^v	105.3 (15)
O2^v—O2—O1^v	59.28 (2)	O2^xiii—O3—H^v	16.1 (15)
S—O2—O3^ix	106.74 (4)	O2ⁱⁱⁱ—O3—H^v	118.9 (15)
Ni—O2—O3^ix	122.74 (3)	O1ⁱⁱ—O3—H^v	74.7 (15)
O1—O2—O3^ix	72.69 (3)	O1^vii—O3—H^v	146.2 (15)
O2^v—O2—O3^ix	129.78 (3)	O2^xiv—O3—H^v	90.3 (15)
O1^v—O2—O3^ix	111.76 (3)	O2ⁱ—O3—H^v	71.6 (15)
S—O2—O1ⁱⁱⁱ	160.48 (4)	O2—O3—H^v	136.1 (15)
Ni—O2—O1ⁱⁱⁱ	47.48 (2)	O2^v—O3—H^v	111.5 (15)
O1—O2—O1ⁱⁱⁱ	138.31 (3)	O1^xiii—O3—H^v	65.4 (15)
O2^v—O2—O1ⁱⁱⁱ	127.67 (2)	O1ⁱⁱⁱ—O3—H^v	131.8 (15)
O1^v—O2—O1ⁱⁱⁱ	161.46 (4)	H—O3—H^v	107 (3)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x, −y+1, z−1/2; (v) −x, y, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) −x, −y, −z+1; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.82 (2)	1.89 (2)	2.6667 (8)	157 (2)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(NiSO4H2O_N2_153K) top

Crystal data top

H₂NiO₅S	V = 341.77 (9) Å³
M_r = 172.79	Z = 4
Monoclinic, C2/c	F(000) = 344
a = 6.8069 (10) Å	D_x = 3.358 Mg m⁻³
b = 7.6152 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.4398 (10) Å	µ = 6.16 mm⁻¹
β = 117.597 (10)°	T = 153 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.023
T_min = 0.657, T_max = 0.748	θ_max = 40.0°, θ_min = 4.3°
10730 measured reflections	h = −12→12
1062 independent reflections	k = −13→13
1034 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.016	w = 1/[σ²(F_o²) + (0.021P)² + 0.480P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.041	(Δ/σ)_max < 0.001
S = 1.11	Δρ_max = 0.78 e Å⁻³
1062 reflections	Δρ_min = −0.68 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0198 (12)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ni	0.000000	0.500000	0.000000	0.00357 (5)
S	0.000000	0.15750 (3)	0.250000	0.00344 (5)
O1	0.17263 (10)	0.04756 (9)	0.40448 (9)	0.00712 (10)
O2	0.10474 (10)	0.27084 (8)	0.15537 (9)	0.00604 (9)
O3	0.000000	0.63067 (11)	0.250000	0.00555 (12)
H	0.109 (3)	0.695 (3)	0.294 (3)	0.018 (5)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni	0.00321 (6)	0.00392 (7)	0.00349 (6)	−0.00011 (3)	0.00146 (4)	0.00013 (3)
S	0.00269 (9)	0.00365 (9)	0.00388 (9)	0.000	0.00144 (7)	0.000
O1	0.0044 (2)	0.0084 (2)	0.0080 (2)	0.00214 (17)	0.00232 (17)	0.00384 (17)
O2	0.0058 (2)	0.0057 (2)	0.0079 (2)	0.00046 (16)	0.00435 (17)	0.00231 (16)
O3	0.0050 (3)	0.0062 (3)	0.0054 (3)	0.000	0.0024 (2)	0.000

Geometric parameters (Å, º) top

Ni—O2ⁱ	2.0313 (6)	O1—O1^v	2.4087 (13)
Ni—O2	2.0313 (6)	O1—O2^v	2.4239 (9)
Ni—O1ⁱⁱ	2.0334 (7)	O1—O2^vi	2.7496 (9)
Ni—O1ⁱⁱⁱ	2.0334 (7)	O1—O3^vii	2.8476 (8)
Ni—O3ⁱ	2.1094 (5)	O1—O2^viii	2.9935 (10)
Ni—O3	2.1094 (5)	O1—O3^ix	3.0100 (7)
Ni—O2ⁱⁱ	3.4170 (7)	O1—O2^vii	3.2148 (10)
Ni—O2ⁱⁱⁱ	3.4170 (7)	O1—O2^x	3.2212 (9)
Ni—O2^iv	3.4382 (7)	O1—O1^xi	3.3411 (13)
Ni—O2^v	3.4382 (7)	O2—O2^v	2.4241 (12)
S—O1^v	1.4668 (6)	O2—O3^ix	2.6682 (8)
S—O1	1.4668 (6)	O2—O3ⁱ	2.8590 (7)
S—O2	1.4879 (6)	O2—O3	2.9962 (11)
S—O2^v	1.4880 (6)	O3—H	0.821 (19)
O1—O2	2.3971 (9)	O3—H^v	0.821 (19)

O2ⁱ—Ni—O2	180.0	O3^ix—O2—O1ⁱⁱⁱ	77.60 (3)
O2ⁱ—Ni—O1ⁱⁱ	85.14 (3)	S—O2—O3ⁱ	135.34 (4)
O2—Ni—O1ⁱⁱ	94.86 (3)	Ni—O2—O3ⁱ	47.48 (2)
O2ⁱ—Ni—O1ⁱⁱⁱ	94.86 (3)	O1—O2—O3ⁱ	150.02 (4)
O2—Ni—O1ⁱⁱⁱ	85.14 (3)	O1^v—O2—O3ⁱ	101.41 (3)
O1ⁱⁱ—Ni—O1ⁱⁱⁱ	180.0	O2^v—O2—O3ⁱ	133.35 (4)
O2ⁱ—Ni—O3ⁱ	92.69 (3)	O3^ix—O2—O3ⁱ	96.40 (2)
O2—Ni—O3ⁱ	87.31 (3)	O1ⁱⁱⁱ—O2—O3ⁱ	60.99 (2)
O1ⁱⁱ—Ni—O3ⁱ	93.18 (2)	S—O2—O1ⁱⁱ	90.87 (3)
O1ⁱⁱⁱ—Ni—O3ⁱ	86.82 (2)	Ni—O2—O1ⁱⁱ	42.596 (17)
O2ⁱ—Ni—O3	87.31 (3)	O1—O2—O1ⁱⁱ	126.27 (3)
O2—Ni—O3	92.69 (3)	O1^v—O2—O1ⁱⁱ	75.69 (3)
O1ⁱⁱ—Ni—O3	86.82 (2)	O2^v—O2—O1ⁱⁱ	71.93 (3)
O1ⁱⁱⁱ—Ni—O3	93.18 (2)	O3^ix—O2—O1ⁱⁱ	158.24 (3)
O3ⁱ—Ni—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.06 (3)
O2ⁱ—Ni—O2ⁱⁱ	98.324 (15)	O3ⁱ—O2—O1ⁱⁱ	61.85 (2)
O2—Ni—O2ⁱⁱ	81.676 (14)	S—O2—O3	101.60 (3)
O1ⁱⁱ—Ni—O2ⁱⁱ	43.59 (2)	Ni—O2—O3	44.688 (15)
O1ⁱⁱⁱ—Ni—O2ⁱⁱ	136.41 (2)	O1—O2—O3	116.66 (3)
O3ⁱ—Ni—O2ⁱⁱ	51.336 (16)	O1^v—O2—O3	115.77 (3)
O3—Ni—O2ⁱⁱ	128.665 (16)	O2^v—O2—O3	66.140 (14)
O2ⁱ—Ni—O2ⁱⁱⁱ	81.675 (14)	O3^ix—O2—O3	128.64 (3)
O2—Ni—O2ⁱⁱⁱ	98.324 (14)	O1ⁱⁱⁱ—O2—O3	63.01 (2)
O1ⁱⁱ—Ni—O2ⁱⁱⁱ	136.41 (2)	O3ⁱ—O2—O3	92.16 (2)
O1ⁱⁱⁱ—Ni—O2ⁱⁱⁱ	43.59 (2)	O1ⁱⁱ—O2—O3	56.772 (17)
O3ⁱ—Ni—O2ⁱⁱⁱ	128.664 (16)	S—O2—O1^vii	82.57 (3)
O3—Ni—O2ⁱⁱⁱ	51.336 (16)	Ni—O2—O1^vii	94.91 (3)
O2ⁱⁱ—Ni—O2ⁱⁱⁱ	180.0	O1—O2—O1^vii	71.73 (3)
O2ⁱ—Ni—O2^iv	43.86 (2)	O1^v—O2—O1^vii	116.64 (3)
O2—Ni—O2^iv	136.14 (2)	O2^v—O2—O1^vii	62.28 (3)
O1ⁱⁱ—Ni—O2^iv	113.71 (2)	O3^ix—O2—O1^vii	87.79 (2)
O1ⁱⁱⁱ—Ni—O2^iv	66.29 (2)	O1ⁱⁱⁱ—O2—O1^vii	78.47 (2)
O3ⁱ—Ni—O2^iv	59.81 (2)	O3ⁱ—O2—O1^vii	136.99 (3)
O3—Ni—O2^iv	120.19 (2)	O1ⁱⁱ—O2—O1^vii	107.45 (3)
O2ⁱⁱ—Ni—O2^iv	96.315 (18)	O3—O2—O1^vii	54.440 (16)
O2ⁱⁱⁱ—Ni—O2^iv	83.685 (18)	S—O2—O1^xii	93.80 (3)
O2ⁱ—Ni—O2^v	136.14 (2)	Ni—O2—O1^xii	115.07 (3)
O2—Ni—O2^v	43.86 (2)	O1—O2—O1^xii	83.46 (2)
O1ⁱⁱ—Ni—O2^v	66.29 (2)	O1^v—O2—O1^xii	70.98 (3)
O1ⁱⁱⁱ—Ni—O2^v	113.71 (2)	O2^v—O2—O1^xii	128.13 (2)
O3ⁱ—Ni—O2^v	120.19 (2)	O3^ix—O2—O1^xii	56.90 (2)
O3—Ni—O2^v	59.81 (2)	O1ⁱⁱⁱ—O2—O1^xii	104.20 (3)
O2ⁱⁱ—Ni—O2^v	83.685 (18)	O3ⁱ—O2—O1^xii	67.59 (3)
O2ⁱⁱⁱ—Ni—O2^v	96.315 (18)	O1ⁱⁱ—O2—O1^xii	110.47 (3)
O2^iv—Ni—O2^v	180.000 (12)	O3—O2—O1^xii	159.75 (3)
O1^v—S—O1	110.39 (6)	O1^vii—O2—O1^xii	141.96 (2)
O1^v—S—O2	110.24 (4)	Ni—O3—Ni^v	123.71 (4)
O1—S—O2	108.44 (3)	Ni—O3—O2^xiii	111.589 (16)
O1^v—S—O2^v	108.44 (3)	Ni^v—O3—O2^xiii	90.545 (16)
O1—S—O2^v	110.24 (4)	Ni—O3—O2ⁱⁱⁱ	90.545 (16)
O2—S—O2^v	109.09 (5)	Ni^v—O3—O2ⁱⁱⁱ	111.589 (17)
S—O1—Ni^vi	136.55 (4)	O2^xiii—O3—O2ⁱⁱⁱ	132.84 (4)
S—O1—O2	36.08 (2)	Ni—O3—O1ⁱⁱ	45.478 (17)
Ni^vi—O1—O2	100.61 (3)	Ni^v—O3—O1ⁱⁱ	104.56 (3)
S—O1—O1^v	34.81 (3)	O2^xiii—O3—O1ⁱⁱ	71.38 (2)
Ni^vi—O1—O1^v	139.49 (4)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	134.48 (2)
O2—O1—O1^v	60.58 (3)	Ni—O3—O1^vii	104.56 (3)
S—O1—O2^v	35.17 (2)	Ni^v—O3—O1^vii	45.478 (17)
Ni^vi—O1—O2^v	145.43 (4)	O2^xiii—O3—O1^vii	134.48 (2)
O2—O1—O2^v	60.37 (3)	O2ⁱⁱⁱ—O3—O1^vii	71.38 (2)
O1^v—O1—O2^v	59.47 (2)	O1ⁱⁱ—O3—O1^vii	123.07 (4)
S—O1—O2^vi	127.75 (4)	Ni—O3—O2^xiv	162.17 (3)
Ni^vi—O1—O2^vi	47.399 (19)	Ni^v—O3—O2^xiv	45.211 (15)
O2—O1—O2^vi	109.98 (3)	O2^xiii—O3—O2^xiv	84.35 (2)
O1^v—O1—O2^vi	102.29 (3)	O2ⁱⁱⁱ—O3—O2^xiv	83.60 (2)
O2^v—O1—O2^vi	161.57 (4)	O1ⁱⁱ—O3—O2^xiv	141.79 (2)
S—O1—O3^vii	170.85 (4)	O1^vii—O3—O2^xiv	57.61 (2)
Ni^vi—O1—O3^vii	47.701 (15)	Ni—O3—O2ⁱ	45.211 (15)
O2—O1—O3^vii	145.69 (3)	Ni^v—O3—O2ⁱ	162.17 (3)
O1^v—O1—O3^vii	150.58 (2)	O2^xiii—O3—O2ⁱ	83.60 (2)
O2^v—O1—O3^vii	135.84 (3)	O2ⁱⁱⁱ—O3—O2ⁱ	84.35 (2)
O2^vi—O1—O3^vii	61.40 (2)	O1ⁱⁱ—O3—O2ⁱ	57.61 (2)
S—O1—O2^viii	115.09 (4)	O1^vii—O3—O2ⁱ	141.79 (2)
Ni^vi—O1—O2^viii	42.541 (19)	O2^xiv—O3—O2ⁱ	149.58 (4)
O2—O1—O2^viii	86.34 (2)	Ni—O3—O2	42.625 (19)
O1^v—O1—O2^viii	146.88 (3)	Ni^v—O3—O2	82.70 (3)
O2^v—O1—O2^viii	104.31 (3)	O2^xiii—O3—O2	128.64 (3)
O2^vi—O1—O2^viii	89.94 (3)	O2ⁱⁱⁱ—O3—O2	96.158 (17)
O3^vii—O1—O2^viii	61.66 (2)	O1ⁱⁱ—O3—O2	61.57 (2)
S—O1—O3^ix	92.69 (3)	O1^vii—O3—O2	66.69 (3)
Ni^vi—O1—O3^ix	44.405 (16)	O2^xiv—O3—O2	121.17 (3)
O2—O1—O3^ix	57.81 (2)	O2ⁱ—O3—O2	87.84 (2)
O1^v—O1—O3^ix	101.73 (4)	Ni—O3—O2^v	82.70 (3)
O2^v—O1—O3^ix	115.71 (3)	Ni^v—O3—O2^v	42.625 (19)
O2^vi—O1—O3^ix	62.50 (3)	O2^xiii—O3—O2^v	96.157 (17)
O3^vii—O1—O3^ix	92.11 (2)	O2ⁱⁱⁱ—O3—O2^v	128.64 (3)
O2^viii—O1—O3^ix	56.88 (2)	O1ⁱⁱ—O3—O2^v	66.69 (3)
S—O1—O2^vii	112.40 (4)	O1^vii—O3—O2^v	61.57 (2)
Ni^vi—O1—O2^vii	78.31 (2)	O2^xiv—O3—O2^v	87.84 (2)
O2—O1—O2^vii	108.27 (3)	O2ⁱ—O3—O2^v	121.17 (3)
O1^v—O1—O2^vii	139.75 (3)	O2—O3—O2^v	47.72 (3)
O2^v—O1—O2^vii	81.07 (2)	Ni—O3—O1^xiii	122.68 (3)
O2^vi—O1—O2^vii	117.36 (3)	Ni^v—O3—O1^xiii	42.416 (14)
O3^vii—O1—O2^vii	58.87 (2)	O2^xiii—O3—O1^xiii	49.494 (18)
O2^viii—O1—O2^vii	45.79 (2)	O2ⁱⁱⁱ—O3—O1^xiii	144.86 (2)
O3^ix—O1—O2^vii	102.44 (2)	O1ⁱⁱ—O3—O1^xiii	80.58 (2)
S—O1—O2^x	127.29 (4)	O1^vii—O3—O1^xiii	87.89 (2)
Ni^vi—O1—O2^x	95.25 (2)	O2^xiv—O3—O1^xiii	61.271 (19)
O2—O1—O2^x	162.54 (4)	O2ⁱ—O3—O1^xiii	126.227 (19)
O1^v—O1—O2^x	102.39 (3)	O2—O3—O1^xiii	101.32 (3)
O2^v—O1—O2^x	109.02 (3)	O2^v—O3—O1^xiii	54.490 (19)
O2^vi—O1—O2^x	75.80 (3)	Ni—O3—O1ⁱⁱⁱ	42.416 (14)
O3^vii—O1—O2^x	51.717 (19)	Ni^v—O3—O1ⁱⁱⁱ	122.68 (3)
O2^viii—O1—O2^x	110.47 (3)	O2^xiii—O3—O1ⁱⁱⁱ	144.86 (2)
O3^ix—O1—O2^x	135.22 (3)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	49.494 (18)
O2^vii—O1—O2^x	81.953 (19)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	87.89 (2)
S—O1—O1^xi	89.49 (3)	O1^vii—O3—O1ⁱⁱⁱ	80.58 (2)
Ni^vi—O1—O1^xi	133.29 (4)	O2^xiv—O3—O1ⁱⁱⁱ	126.227 (19)
O2—O1—O1^xi	124.13 (4)	O2ⁱ—O3—O1ⁱⁱⁱ	61.271 (19)
O1^v—O1—O1^xi	80.70 (3)	O2—O3—O1ⁱⁱⁱ	54.490 (19)
O2^v—O1—O1^xi	65.71 (3)	O2^v—O3—O1ⁱⁱⁱ	101.32 (3)
O2^vi—O1—O1^xi	116.86 (3)	O1^xiii—O3—O1ⁱⁱⁱ	155.72 (4)
O3^vii—O1—O1^xi	85.59 (3)	Ni—O3—H	105.2 (14)
O2^viii—O1—O1^xi	121.10 (3)	Ni^v—O3—H	107.5 (14)
O3^ix—O1—O1^xi	177.56 (3)	O2^xiii—O3—H	118.8 (14)
O2^vii—O1—O1^xi	75.67 (3)	O2ⁱⁱⁱ—O3—H	16.3 (14)
O2^x—O1—O1^xi	43.305 (19)	O1ⁱⁱ—O3—H	146.0 (14)
S—O2—Ni	130.45 (4)	O1^vii—O3—H	75.0 (14)
S—O2—O1	35.48 (2)	O2^xiv—O3—H	71.7 (14)
Ni—O2—O1	160.13 (4)	O2ⁱ—O3—H	90.0 (14)
S—O2—O1^v	34.60 (2)	O2—O3—H	111.7 (14)
Ni—O2—O1^v	117.38 (3)	O2^v—O3—H	136.3 (14)
O1—O2—O1^v	59.95 (3)	O1^xiii—O3—H	131.9 (14)
S—O2—O2^v	35.46 (3)	O1ⁱⁱⁱ—O3—H	65.4 (14)
Ni—O2—O2^v	100.65 (2)	Ni—O3—H^v	107.5 (14)
O1—O2—O2^v	60.36 (2)	Ni^v—O3—H^v	105.2 (14)
O1^v—O2—O2^v	59.27 (2)	O2^xiii—O3—H^v	16.3 (14)
S—O2—O3^ix	106.78 (3)	O2ⁱⁱⁱ—O3—H^v	118.8 (14)
Ni—O2—O3^ix	122.62 (3)	O1ⁱⁱ—O3—H^v	75.0 (14)
O1—O2—O3^ix	72.69 (3)	O1^vii—O3—H^v	146.0 (14)
O1^v—O2—O3^ix	111.85 (3)	O2^xiv—O3—H^v	90.0 (14)
O2^v—O2—O3^ix	129.74 (3)	O2ⁱ—O3—H^v	71.7 (14)
S—O2—O1ⁱⁱⁱ	160.39 (4)	O2—O3—H^v	136.3 (14)
Ni—O2—O1ⁱⁱⁱ	47.46 (2)	O2^v—O3—H^v	111.7 (14)
O1—O2—O1ⁱⁱⁱ	138.20 (3)	O1^xiii—O3—H^v	65.4 (14)
O1^v—O2—O1ⁱⁱⁱ	161.57 (4)	O1ⁱⁱⁱ—O3—H^v	131.9 (14)
O2^v—O2—O1ⁱⁱⁱ	127.64 (2)	H—O3—H^v	107 (3)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x, −y+1, z−1/2; (v) −x, y, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) −x, −y, −z+1; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.821 (19)	1.894 (19)	2.6681 (8)	157 (2)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(NiSO4H2O_N2_193K) top

Crystal data top

H₂NiO₅S	V = 341.98 (9) Å³
M_r = 172.79	Z = 4
Monoclinic, C2/c	F(000) = 344
a = 6.8115 (10) Å	D_x = 3.356 Mg m⁻³
b = 7.6122 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.4444 (10) Å	µ = 6.16 mm⁻¹
β = 117.629 (10)°	T = 193 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.023
T_min = 0.646, T_max = 0.748	θ_max = 40.0°, θ_min = 4.3°
10714 measured reflections	h = −12→12
1063 independent reflections	k = −13→13
1036 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.016	w = 1/[σ²(F_o²) + (0.021P)² + 0.470P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.042	(Δ/σ)_max < 0.001
S = 1.12	Δρ_max = 0.80 e Å⁻³
1063 reflections	Δρ_min = −0.72 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0206 (13)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ni	0.000000	0.500000	0.000000	0.00428 (5)
S	0.000000	0.15727 (3)	0.250000	0.00404 (5)
O1	0.17262 (10)	0.04732 (9)	0.40413 (10)	0.00843 (10)
O2	0.10428 (10)	0.27059 (8)	0.15519 (9)	0.00703 (9)
O3	0.000000	0.63077 (12)	0.250000	0.00631 (12)
H	0.109 (3)	0.695 (3)	0.294 (3)	0.020 (5)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni	0.00390 (6)	0.00468 (7)	0.00412 (6)	−0.00014 (4)	0.00173 (5)	0.00016 (3)
S	0.00314 (9)	0.00423 (10)	0.00453 (9)	0.000	0.00159 (7)	0.000
O1	0.0052 (2)	0.0100 (2)	0.0094 (2)	0.00250 (18)	0.00281 (18)	0.00463 (18)
O2	0.0067 (2)	0.0066 (2)	0.0094 (2)	0.00068 (16)	0.00512 (18)	0.00264 (16)
O3	0.0060 (3)	0.0070 (3)	0.0061 (3)	0.000	0.0029 (2)	0.000

Geometric parameters (Å, º) top

Ni—O2	2.0317 (6)	O1—O1^v	2.4065 (13)
Ni—O2ⁱ	2.0317 (6)	O1—O2^v	2.4225 (9)
Ni—O1ⁱⁱ	2.0336 (7)	O1—O2^vi	2.7503 (9)
Ni—O1ⁱⁱⁱ	2.0336 (7)	O1—O3^vii	2.8486 (8)
Ni—O3ⁱ	2.1106 (5)	O1—O2^viii	2.9938 (10)
Ni—O3	2.1106 (5)	O1—O3^ix	3.0110 (7)
Ni—O2ⁱⁱ	3.4176 (7)	O1—O2^vii	3.2200 (10)
Ni—O2ⁱⁱⁱ	3.4176 (7)	O1—O2^x	3.2208 (10)
Ni—O2^iv	3.4401 (7)	O1—O1^xi	3.3466 (13)
Ni—O2^v	3.4401 (7)	O2—O2^v	2.4229 (12)
S—O1	1.4657 (7)	O2—O3^ix	2.6706 (8)
S—O1^v	1.4657 (7)	O2—O3ⁱ	2.8601 (8)
S—O2^v	1.4872 (6)	O2—O3	2.9975 (11)
S—O2	1.4872 (6)	O3—H	0.82 (2)
O1—O2	2.3957 (9)	O3—H^v	0.82 (2)

O2—Ni—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	77.44 (3)
O2—Ni—O1ⁱⁱ	94.85 (3)	S—O2—O3ⁱ	135.49 (4)
O2ⁱ—Ni—O1ⁱⁱ	85.15 (3)	Ni—O2—O3ⁱ	47.49 (2)
O2—Ni—O1ⁱⁱⁱ	85.15 (3)	O1—O2—O3ⁱ	150.02 (4)
O2ⁱ—Ni—O1ⁱⁱⁱ	94.85 (3)	O1^v—O2—O3ⁱ	101.56 (3)
O1ⁱⁱ—Ni—O1ⁱⁱⁱ	180.00 (4)	O2^v—O2—O3ⁱ	133.51 (4)
O2—Ni—O3ⁱ	87.31 (3)	O3^ix—O2—O3ⁱ	96.31 (2)
O2ⁱ—Ni—O3ⁱ	92.69 (3)	O1ⁱⁱⁱ—O2—O3ⁱ	60.99 (2)
O1ⁱⁱ—Ni—O3ⁱ	93.18 (2)	S—O2—O1ⁱⁱ	91.02 (3)
O1ⁱⁱⁱ—Ni—O3ⁱ	86.82 (2)	Ni—O2—O1ⁱⁱ	42.599 (18)
O2—Ni—O3	92.69 (3)	O1—O2—O1ⁱⁱ	126.41 (4)
O2ⁱ—Ni—O3	87.31 (3)	O1^v—O2—O1ⁱⁱ	75.80 (3)
O1ⁱⁱ—Ni—O3	86.82 (2)	O2^v—O2—O1ⁱⁱ	72.08 (3)
O1ⁱⁱⁱ—Ni—O3	93.18 (2)	O3^ix—O2—O1ⁱⁱ	158.16 (3)
O3ⁱ—Ni—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.06 (3)
O2—Ni—O2ⁱⁱ	81.665 (14)	O3ⁱ—O2—O1ⁱⁱ	61.86 (2)
O2ⁱ—Ni—O2ⁱⁱ	98.335 (15)	S—O2—O3	101.61 (3)
O1ⁱⁱ—Ni—O2ⁱⁱ	43.54 (2)	Ni—O2—O3	44.697 (16)
O1ⁱⁱⁱ—Ni—O2ⁱⁱ	136.46 (2)	O1—O2—O3	116.68 (3)
O3ⁱ—Ni—O2ⁱⁱ	51.388 (16)	O1^v—O2—O3	115.80 (3)
O3—Ni—O2ⁱⁱ	128.612 (16)	O2^v—O2—O3	66.162 (14)
O2—Ni—O2ⁱⁱⁱ	98.335 (15)	O3^ix—O2—O3	128.51 (3)
O2ⁱ—Ni—O2ⁱⁱⁱ	81.665 (15)	O1ⁱⁱⁱ—O2—O3	63.01 (2)
O1ⁱⁱ—Ni—O2ⁱⁱⁱ	136.46 (2)	O3ⁱ—O2—O3	92.19 (2)
O1ⁱⁱⁱ—Ni—O2ⁱⁱⁱ	43.54 (2)	O1ⁱⁱ—O2—O3	56.780 (17)
O3ⁱ—Ni—O2ⁱⁱⁱ	128.612 (16)	S—O2—O1^vii	82.52 (3)
O3—Ni—O2ⁱⁱⁱ	51.388 (16)	Ni—O2—O1^vii	94.86 (3)
O2ⁱⁱ—Ni—O2ⁱⁱⁱ	180.00 (2)	O1—O2—O1^vii	71.74 (3)
O2—Ni—O2^iv	136.21 (2)	O1^v—O2—O1^vii	116.58 (3)
O2ⁱ—Ni—O2^iv	43.79 (2)	O2^v—O2—O1^vii	62.20 (3)
O1ⁱⁱ—Ni—O2^iv	113.60 (2)	O3^ix—O2—O1^vii	87.75 (2)
O1ⁱⁱⁱ—Ni—O2^iv	66.40 (2)	O1ⁱⁱⁱ—O2—O1^vii	78.41 (2)
O3ⁱ—Ni—O2^iv	59.80 (3)	O3ⁱ—O2—O1^vii	136.93 (3)
O3—Ni—O2^iv	120.20 (3)	O1ⁱⁱ—O2—O1^vii	107.43 (3)
O2ⁱⁱ—Ni—O2^iv	96.280 (19)	O3—O2—O1^vii	54.395 (17)
O2ⁱⁱⁱ—Ni—O2^iv	83.720 (19)	S—O2—O1^xii	93.95 (3)
O2—Ni—O2^v	43.79 (2)	Ni—O2—O1^xii	114.98 (3)
O2ⁱ—Ni—O2^v	136.21 (2)	O1—O2—O1^xii	83.53 (2)
O1ⁱⁱ—Ni—O2^v	66.40 (2)	O1^v—O2—O1^xii	71.15 (3)
O1ⁱⁱⁱ—Ni—O2^v	113.60 (2)	O2^v—O2—O1^xii	128.29 (2)
O3ⁱ—Ni—O2^v	120.20 (3)	O3^ix—O2—O1^xii	56.91 (2)
O3—Ni—O2^v	59.80 (3)	O1ⁱⁱⁱ—O2—O1^xii	104.06 (3)
O2ⁱⁱ—Ni—O2^v	83.720 (19)	O3ⁱ—O2—O1^xii	67.50 (3)
O2ⁱⁱⁱ—Ni—O2^v	96.280 (19)	O1ⁱⁱ—O2—O1^xii	110.49 (3)
O2^iv—Ni—O2^v	180.0	O3—O2—O1^xii	159.67 (3)
O1—S—O1^v	110.36 (6)	O1^vii—O2—O1^xii	141.97 (2)
O1—S—O2^v	110.24 (4)	Ni—O3—Ni^v	123.72 (4)
O1^v—S—O2^v	108.45 (4)	Ni—O3—O2^xiii	111.572 (17)
O1—S—O2	108.45 (4)	Ni^v—O3—O2^xiii	90.474 (16)
O1^v—S—O2	110.24 (4)	Ni—O3—O2ⁱⁱⁱ	90.475 (16)
O2^v—S—O2	109.10 (5)	Ni^v—O3—O2ⁱⁱⁱ	111.572 (17)
S—O1—Ni^vi	136.63 (4)	O2^xiii—O3—O2ⁱⁱⁱ	133.02 (5)
S—O1—O2	36.08 (2)	Ni—O3—O1ⁱⁱ	45.464 (17)
Ni^vi—O1—O2	100.67 (3)	Ni^v—O3—O1ⁱⁱ	104.62 (3)
S—O1—O1^v	34.82 (3)	O2^xiii—O3—O1ⁱⁱ	71.32 (2)
Ni^vi—O1—O1^v	139.66 (5)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	134.40 (2)
O2—O1—O1^v	60.59 (3)	Ni—O3—O1^vii	104.62 (3)
S—O1—O2^v	35.17 (2)	Ni^v—O3—O1^vii	45.464 (17)
Ni^vi—O1—O2^v	145.34 (4)	O2^xiii—O3—O1^vii	134.40 (2)
O2—O1—O2^v	60.38 (3)	O2ⁱⁱⁱ—O3—O1^vii	71.32 (2)
O1^v—O1—O2^v	59.48 (3)	O1ⁱⁱ—O3—O1^vii	123.16 (4)
S—O1—O2^vi	127.88 (4)	Ni—O3—O2^xiv	162.22 (3)
Ni^vi—O1—O2^vi	47.397 (19)	Ni^v—O3—O2^xiv	45.201 (15)
O2—O1—O2^vi	110.05 (3)	O2^xiii—O3—O2^xiv	84.30 (2)
O1^v—O1—O2^vi	102.43 (3)	O2ⁱⁱⁱ—O3—O2^xiv	83.69 (2)
O2^v—O1—O2^vi	161.72 (4)	O1ⁱⁱ—O3—O2^xiv	141.78 (2)
S—O1—O3^vii	170.71 (4)	O1^vii—O3—O2^xiv	57.60 (2)
Ni^vi—O1—O3^vii	47.713 (15)	Ni—O3—O2ⁱ	45.201 (15)
O2—O1—O3^vii	145.75 (3)	Ni^v—O3—O2ⁱ	162.22 (3)
O1^v—O1—O3^vii	150.59 (2)	O2^xiii—O3—O2ⁱ	83.69 (2)
O2^v—O1—O3^vii	135.69 (3)	O2ⁱⁱⁱ—O3—O2ⁱ	84.30 (2)
O2^vi—O1—O3^vii	61.41 (2)	O1ⁱⁱ—O3—O2ⁱ	57.60 (2)
S—O1—O2^viii	115.05 (4)	O1^vii—O3—O2ⁱ	141.78 (2)
Ni^vi—O1—O2^viii	42.548 (19)	O2^xiv—O3—O2ⁱ	149.56 (4)
O2—O1—O2^viii	86.37 (3)	Ni—O3—O2	42.614 (19)
O1^v—O1—O2^viii	146.91 (3)	Ni^v—O3—O2	82.71 (3)
O2^v—O1—O2^viii	104.20 (3)	O2^xiii—O3—O2	128.51 (3)
O2^vi—O1—O2^viii	89.95 (3)	O2ⁱⁱⁱ—O3—O2	96.110 (18)
O3^vii—O1—O2^viii	61.68 (3)	O1ⁱⁱ—O3—O2	61.54 (2)
S—O1—O3^ix	92.76 (3)	O1^vii—O3—O2	66.79 (3)
Ni^vi—O1—O3^ix	44.418 (17)	O2^xiv—O3—O2	121.22 (3)
O2—O1—O3^ix	57.87 (2)	O2ⁱ—O3—O2	87.81 (2)
O1^v—O1—O3^ix	101.86 (4)	Ni—O3—O2^v	82.71 (3)
O2^v—O1—O3^ix	115.73 (3)	Ni^v—O3—O2^v	42.614 (19)
O2^vi—O1—O3^ix	62.51 (3)	O2^xiii—O3—O2^v	96.109 (18)
O3^vii—O1—O3^ix	92.13 (2)	O2ⁱⁱⁱ—O3—O2^v	128.51 (3)
O2^viii—O1—O3^ix	56.89 (2)	O1ⁱⁱ—O3—O2^v	66.79 (3)
S—O1—O2^vii	112.33 (4)	O1^vii—O3—O2^v	61.54 (2)
Ni^vi—O1—O2^vii	78.24 (2)	O2^xiv—O3—O2^v	87.82 (2)
O2—O1—O2^vii	108.26 (3)	O2ⁱ—O3—O2^v	121.22 (3)
O1^v—O1—O2^vii	139.67 (3)	O2—O3—O2^v	47.68 (3)
O2^v—O1—O2^vii	80.99 (3)	Ni—O3—O1^xiii	122.64 (3)
O2^vi—O1—O2^vii	117.29 (3)	Ni^v—O3—O1^xiii	42.405 (14)
O3^vii—O1—O2^vii	58.82 (2)	O2^xiii—O3—O1^xiii	49.435 (19)
O2^viii—O1—O2^vii	45.72 (2)	O2ⁱⁱⁱ—O3—O1^xiii	144.93 (2)
O3^ix—O1—O2^vii	102.38 (3)	O1ⁱⁱ—O3—O1^xiii	80.58 (2)
S—O1—O2^x	127.16 (4)	O1^vii—O3—O1^xiii	87.87 (2)
Ni^vi—O1—O2^x	95.35 (3)	O2^xiv—O3—O1^xiii	61.25 (2)
O2—O1—O2^x	162.44 (4)	O2ⁱ—O3—O1^xiii	126.28 (2)
O1^v—O1—O2^x	102.30 (3)	O2—O3—O1^xiii	101.25 (3)
O2^v—O1—O2^x	108.85 (3)	O2^v—O3—O1^xiii	54.48 (2)
O2^vi—O1—O2^x	75.94 (3)	Ni—O3—O1ⁱⁱⁱ	42.405 (14)
O3^vii—O1—O2^x	51.77 (2)	Ni^v—O3—O1ⁱⁱⁱ	122.64 (3)
O2^viii—O1—O2^x	110.49 (3)	O2^xiii—O3—O1ⁱⁱⁱ	144.93 (2)
O3^ix—O1—O2^x	135.36 (3)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	49.435 (19)
O2^vii—O1—O2^x	81.903 (19)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	87.87 (2)
S—O1—O1^xi	89.40 (3)	O1^vii—O3—O1ⁱⁱⁱ	80.58 (2)
Ni^vi—O1—O1^xi	133.25 (4)	O2^xiv—O3—O1ⁱⁱⁱ	126.28 (2)
O2—O1—O1^xi	124.04 (4)	O2ⁱ—O3—O1ⁱⁱⁱ	61.25 (2)
O1^v—O1—O1^xi	80.65 (4)	O2—O3—O1ⁱⁱⁱ	54.48 (2)
O2^v—O1—O1^xi	65.61 (3)	O2^v—O3—O1ⁱⁱⁱ	101.25 (3)
O2^vi—O1—O1^xi	116.97 (4)	O1^xiii—O3—O1ⁱⁱⁱ	155.64 (4)
O3^vii—O1—O1^xi	85.55 (3)	Ni—O3—H	105.2 (15)
O2^viii—O1—O1^xi	120.95 (4)	Ni^v—O3—H	107.3 (14)
O3^ix—O1—O1^xi	177.49 (3)	O2^xiii—O3—H	119.2 (14)
O2^vii—O1—O1^xi	75.59 (3)	O2ⁱⁱⁱ—O3—H	16.2 (14)
O2^x—O1—O1^xi	43.24 (2)	O1ⁱⁱ—O3—H	146.0 (15)
S—O2—Ni	130.57 (4)	O1^vii—O3—H	74.7 (14)
S—O2—O1	35.48 (2)	O2^xiv—O3—H	71.7 (15)
Ni—O2—O1	160.21 (4)	O2ⁱ—O3—H	90.1 (15)
S—O2—O1^v	34.59 (2)	O2—O3—H	111.5 (14)
Ni—O2—O1^v	117.52 (3)	O2^v—O3—H	136.0 (14)
O1—O2—O1^v	59.93 (4)	O1^xiii—O3—H	131.9 (15)
S—O2—O2^v	35.45 (3)	O1ⁱⁱⁱ—O3—H	65.3 (15)
Ni—O2—O2^v	100.75 (2)	Ni—O3—H^v	107.3 (14)
O1—O2—O2^v	60.36 (3)	Ni^v—O3—H^v	105.2 (15)
O1^v—O2—O2^v	59.26 (2)	O2^xiii—O3—H^v	16.2 (15)
S—O2—O3^ix	106.80 (4)	O2ⁱⁱⁱ—O3—H^v	119.2 (14)
Ni—O2—O3^ix	122.46 (3)	O1ⁱⁱ—O3—H^v	74.7 (14)
O1—O2—O3^ix	72.70 (3)	O1^vii—O3—H^v	146.0 (15)
O1^v—O2—O3^ix	111.94 (4)	O2^xiv—O3—H^v	90.1 (15)
O2^v—O2—O3^ix	129.69 (4)	O2ⁱ—O3—H^v	71.7 (15)
S—O2—O1ⁱⁱⁱ	160.31 (4)	O2—O3—H^v	136.0 (14)
Ni—O2—O1ⁱⁱⁱ	47.46 (2)	O2^v—O3—H^v	111.5 (14)
O1—O2—O1ⁱⁱⁱ	138.07 (3)	O1^xiii—O3—H^v	65.3 (15)
O1^v—O2—O1ⁱⁱⁱ	161.72 (4)	O1ⁱⁱⁱ—O3—H^v	131.9 (15)
O2^v—O2—O1ⁱⁱⁱ	127.62 (2)	H—O3—H^v	107 (3)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x, −y+1, z−1/2; (v) −x, y, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) −x, −y, −z+1; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.82 (2)	1.90 (2)	2.6706 (8)	157 (2)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(NiSO4H2O_N2_233K) top

Crystal data top

H₂NiO₅S	V = 342.35 (9) Å³
M_r = 172.79	Z = 4
Monoclinic, C2/c	F(000) = 344
a = 6.8176 (10) Å	D_x = 3.352 Mg m⁻³
b = 7.6098 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.4513 (10) Å	µ = 6.15 mm⁻¹
β = 117.676 (10)°	T = 233 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.024
T_min = 0.670, T_max = 0.748	θ_max = 40.0°, θ_min = 4.3°
10733 measured reflections	h = −12→12
1064 independent reflections	k = −13→13
1033 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.016	w = 1/[σ²(F_o²) + (0.023P)² + 0.4P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.044	(Δ/σ)_max < 0.001
S = 1.13	Δρ_max = 0.85 e Å⁻³
1064 reflections	Δρ_min = −0.68 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0222 (14)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ni	0.000000	0.500000	0.000000	0.00492 (5)
S	0.000000	0.15705 (3)	0.250000	0.00453 (6)
O1	0.17277 (10)	0.04702 (10)	0.40390 (10)	0.00962 (11)
O2	0.10392 (10)	0.27036 (8)	0.15499 (10)	0.00809 (10)
O3	0.000000	0.63099 (12)	0.250000	0.00704 (12)
H	0.109 (3)	0.695 (3)	0.296 (3)	0.018 (4)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni	0.00440 (7)	0.00540 (7)	0.00470 (7)	−0.00017 (4)	0.00190 (5)	0.00020 (3)
S	0.00342 (9)	0.00469 (10)	0.00518 (9)	0.000	0.00173 (7)	0.000
O1	0.0057 (2)	0.0114 (3)	0.0109 (2)	0.00282 (19)	0.00316 (18)	0.00550 (19)
O2	0.0077 (2)	0.0077 (2)	0.0107 (2)	0.00093 (17)	0.00581 (18)	0.00324 (17)
O3	0.0064 (3)	0.0078 (3)	0.0069 (3)	0.000	0.0031 (2)	0.000

Geometric parameters (Å, º) top

Ni—O2	2.0321 (7)	O1—O1^v	2.4064 (13)
Ni—O2ⁱ	2.0321 (7)	O1—O2^v	2.4229 (9)
Ni—O1ⁱⁱ	2.0332 (7)	O1—O2^vi	2.7502 (10)
Ni—O1ⁱⁱⁱ	2.0332 (7)	O1—O3^vii	2.8492 (8)
Ni—O3	2.1127 (5)	O1—O2^viii	2.9939 (10)
Ni—O3ⁱ	2.1128 (5)	O1—O3^ix	3.0128 (8)
Ni—O2ⁱⁱ	3.4183 (7)	O1—O2^x	3.2202 (10)
Ni—O2ⁱⁱⁱ	3.4183 (7)	O1—O2^vii	3.2255 (11)
Ni—O2^iv	3.4433 (7)	O1—O1^xi	3.3536 (14)
Ni—O2^v	3.4433 (7)	O2—O2^v	2.4241 (13)
S—O1^v	1.4659 (7)	O2—O3^ix	2.6724 (8)
S—O1	1.4659 (7)	O2—O3ⁱ	2.8612 (8)
S—O2	1.4874 (6)	O2—O3	3.0000 (11)
S—O2^v	1.4875 (6)	O3—H	0.820 (19)
O1—O2	2.3958 (9)	O3—H^v	0.820 (19)

O2—Ni—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	77.29 (3)
O2—Ni—O1ⁱⁱ	94.86 (3)	S—O2—O3ⁱ	135.62 (4)
O2ⁱ—Ni—O1ⁱⁱ	85.14 (3)	Ni—O2—O3ⁱ	47.53 (2)
O2—Ni—O1ⁱⁱⁱ	85.14 (3)	O1—O2—O3ⁱ	150.01 (4)
O2ⁱ—Ni—O1ⁱⁱⁱ	94.86 (3)	O1^v—O2—O3ⁱ	101.68 (3)
O1ⁱⁱ—Ni—O1ⁱⁱⁱ	180.00 (4)	O2^v—O2—O3ⁱ	133.67 (4)
O2—Ni—O3	92.72 (3)	O3^ix—O2—O3ⁱ	96.21 (2)
O2ⁱ—Ni—O3	87.28 (3)	O1ⁱⁱⁱ—O2—O3ⁱ	60.99 (2)
O1ⁱⁱ—Ni—O3	86.80 (2)	S—O2—O1ⁱⁱ	91.15 (3)
O1ⁱⁱⁱ—Ni—O3	93.20 (2)	Ni—O2—O1ⁱⁱ	42.585 (18)
O2—Ni—O3ⁱ	87.28 (3)	O1—O2—O1ⁱⁱ	126.55 (4)
O2ⁱ—Ni—O3ⁱ	92.72 (3)	O1^v—O2—O1ⁱⁱ	75.91 (3)
O1ⁱⁱ—Ni—O3ⁱ	93.20 (2)	O2^v—O2—O1ⁱⁱ	72.21 (3)
O1ⁱⁱⁱ—Ni—O3ⁱ	86.80 (2)	O3^ix—O2—O1ⁱⁱ	158.08 (3)
O3—Ni—O3ⁱ	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.03 (3)
O2—Ni—O2ⁱⁱ	81.659 (15)	O3ⁱ—O2—O1ⁱⁱ	61.89 (2)
O2ⁱ—Ni—O2ⁱⁱ	98.341 (15)	S—O2—O3	101.60 (3)
O1ⁱⁱ—Ni—O2ⁱⁱ	43.52 (2)	Ni—O2—O3	44.704 (16)
O1ⁱⁱⁱ—Ni—O2ⁱⁱ	136.48 (2)	O1—O2—O3	116.68 (3)
O3—Ni—O2ⁱⁱ	128.576 (16)	O1^v—O2—O3	115.79 (3)
O3ⁱ—Ni—O2ⁱⁱ	51.424 (16)	O2^v—O2—O3	66.172 (14)
O2—Ni—O2ⁱⁱⁱ	98.341 (15)	O3^ix—O2—O3	128.38 (3)
O2ⁱ—Ni—O2ⁱⁱⁱ	81.658 (15)	O1ⁱⁱⁱ—O2—O3	63.02 (2)
O1ⁱⁱ—Ni—O2ⁱⁱⁱ	136.48 (2)	O3ⁱ—O2—O3	92.23 (2)
O1ⁱⁱⁱ—Ni—O2ⁱⁱⁱ	43.52 (2)	O1ⁱⁱ—O2—O3	56.765 (18)
O3—Ni—O2ⁱⁱⁱ	51.425 (16)	S—O2—O1^xii	94.12 (3)
O3ⁱ—Ni—O2ⁱⁱⁱ	128.575 (16)	Ni—O2—O1^xii	114.91 (3)
O2ⁱⁱ—Ni—O2ⁱⁱⁱ	180.0	O1—O2—O1^xii	83.61 (2)
O2—Ni—O2^iv	136.26 (2)	O1^v—O2—O1^xii	71.34 (3)
O2ⁱ—Ni—O2^iv	43.75 (2)	O2^v—O2—O1^xii	128.45 (2)
O1ⁱⁱ—Ni—O2^iv	113.51 (2)	O3^ix—O2—O1^xii	56.92 (2)
O1ⁱⁱⁱ—Ni—O2^iv	66.49 (2)	O1ⁱⁱⁱ—O2—O1^xii	103.92 (3)
O3—Ni—O2^iv	120.20 (3)	O3ⁱ—O2—O1^xii	67.39 (3)
O3ⁱ—Ni—O2^iv	59.80 (3)	O1ⁱⁱ—O2—O1^xii	110.54 (3)
O2ⁱⁱ—Ni—O2^iv	96.233 (19)	O3—O2—O1^xii	159.60 (3)
O2ⁱⁱⁱ—Ni—O2^iv	83.766 (19)	S—O2—O1^vii	82.44 (3)
O2—Ni—O2^v	43.74 (2)	Ni—O2—O1^vii	94.79 (3)
O2ⁱ—Ni—O2^v	136.25 (2)	O1—O2—O1^vii	71.75 (3)
O1ⁱⁱ—Ni—O2^v	66.49 (2)	O1^v—O2—O1^vii	116.49 (3)
O1ⁱⁱⁱ—Ni—O2^v	113.51 (2)	O2^v—O2—O1^vii	62.10 (3)
O3—Ni—O2^v	59.80 (3)	O3^ix—O2—O1^vii	87.73 (2)
O3ⁱ—Ni—O2^v	120.20 (3)	O1ⁱⁱⁱ—O2—O1^vii	78.38 (2)
O2ⁱⁱ—Ni—O2^v	83.767 (19)	O3ⁱ—O2—O1^vii	136.90 (3)
O2ⁱⁱⁱ—Ni—O2^v	96.234 (19)	O1ⁱⁱ—O2—O1^vii	107.37 (3)
O2^iv—Ni—O2^v	180.0	O3—O2—O1^vii	54.327 (17)
O1^v—S—O1	110.33 (6)	O1^xii—O2—O1^vii	142.00 (3)
O1^v—S—O2	110.25 (4)	Ni—O3—Ni^v	123.70 (4)
O1—S—O2	108.43 (4)	Ni—O3—O2^xiii	111.559 (18)
O1^v—S—O2^v	108.43 (4)	Ni^v—O3—O2^xiii	90.401 (16)
O1—S—O2^v	110.25 (4)	Ni—O3—O2ⁱⁱⁱ	90.401 (16)
O2—S—O2^v	109.14 (5)	Ni^v—O3—O2ⁱⁱⁱ	111.560 (18)
S—O1—Ni^vi	136.69 (4)	O2^xiii—O3—O2ⁱⁱⁱ	133.24 (5)
S—O1—O2	36.09 (2)	Ni—O3—O1ⁱⁱ	45.437 (17)
Ni^vi—O1—O2	100.71 (3)	Ni^v—O3—O1ⁱⁱ	104.66 (3)
S—O1—O1^v	34.83 (3)	O2^xiii—O3—O1ⁱⁱ	71.27 (2)
Ni^vi—O1—O1^v	139.81 (5)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	134.30 (2)
O2—O1—O1^v	60.60 (3)	Ni—O3—O1^vii	104.66 (3)
S—O1—O2^v	35.17 (2)	Ni^v—O3—O1^vii	45.437 (17)
Ni^vi—O1—O2^v	145.27 (4)	O2^xiii—O3—O1^vii	134.31 (2)
O2—O1—O2^v	60.40 (3)	O2ⁱⁱⁱ—O3—O1^vii	71.27 (2)
O1^v—O1—O2^v	59.48 (3)	O1ⁱⁱ—O3—O1^vii	123.23 (4)
S—O1—O2^vi	128.00 (4)	Ni—O3—O2^xiv	162.24 (3)
Ni^vi—O1—O2^vi	47.413 (19)	Ni^v—O3—O2^xiv	45.191 (15)
O2—O1—O2^vi	110.09 (3)	O2^xiii—O3—O2^xiv	84.26 (2)
O1^v—O1—O2^vi	102.55 (3)	O2ⁱⁱⁱ—O3—O2^xiv	83.78 (2)
O2^v—O1—O2^vi	161.84 (4)	O1ⁱⁱ—O3—O2^xiv	141.78 (2)
S—O1—O3^vii	170.57 (5)	O1^vii—O3—O2^xiv	57.58 (2)
Ni^vi—O1—O3^vii	47.762 (15)	Ni—O3—O2ⁱ	45.191 (15)
O2—O1—O3^vii	145.84 (3)	Ni^v—O3—O2ⁱ	162.24 (3)
O1^v—O1—O3^vii	150.58 (2)	O2^xiii—O3—O2ⁱ	83.78 (2)
O2^v—O1—O3^vii	135.55 (3)	O2ⁱⁱⁱ—O3—O2ⁱ	84.26 (2)
O2^vi—O1—O3^vii	61.43 (2)	O1ⁱⁱ—O3—O2ⁱ	57.58 (2)
S—O1—O2^viii	115.00 (4)	O1^vii—O3—O2ⁱ	141.78 (2)
Ni^vi—O1—O2^viii	42.557 (19)	O2^xiv—O3—O2ⁱ	149.57 (4)
O2—O1—O2^viii	86.39 (3)	Ni—O3—O2	42.58 (2)
O1^v—O1—O2^viii	146.93 (3)	Ni^v—O3—O2	82.71 (3)
O2^v—O1—O2^viii	104.09 (3)	O2^xiii—O3—O2	128.38 (3)
O2^vi—O1—O2^viii	89.97 (3)	O2ⁱⁱⁱ—O3—O2	96.041 (17)
O3^vii—O1—O2^viii	61.73 (3)	O1ⁱⁱ—O3—O2	61.51 (2)
S—O1—O3^ix	92.81 (3)	O1^vii—O3—O2	66.87 (3)
Ni^vi—O1—O3^ix	44.441 (17)	O2^xiv—O3—O2	121.26 (3)
O2—O1—O3^ix	57.88 (2)	O2ⁱ—O3—O2	87.77 (2)
O1^v—O1—O3^ix	101.97 (4)	Ni—O3—O2^v	82.71 (3)
O2^v—O1—O3^ix	115.73 (3)	Ni^v—O3—O2^v	42.578 (19)
O2^vi—O1—O3^ix	62.55 (3)	O2^xiii—O3—O2^v	96.040 (18)
O3^vii—O1—O3^ix	92.20 (2)	O2ⁱⁱⁱ—O3—O2^v	128.38 (3)
O2^viii—O1—O3^ix	56.89 (2)	O1ⁱⁱ—O3—O2^v	66.87 (3)
S—O1—O2^x	127.01 (4)	O1^vii—O3—O2^v	61.51 (2)
Ni^vi—O1—O2^x	95.49 (3)	O2^xiv—O3—O2^v	87.77 (2)
O2—O1—O2^x	162.33 (4)	O2ⁱ—O3—O2^v	121.26 (3)
O1^v—O1—O2^x	102.20 (3)	O2—O3—O2^v	47.66 (3)
O2^v—O1—O2^x	108.66 (3)	Ni—O3—O1^xiii	122.60 (3)
O2^vi—O1—O2^x	76.08 (3)	Ni^v—O3—O1^xiii	42.361 (14)
O3^vii—O1—O2^x	51.81 (2)	O2^xiii—O3—O1^xiii	49.402 (19)
O2^viii—O1—O2^x	110.54 (3)	O2ⁱⁱⁱ—O3—O1^xiii	144.99 (2)
O3^ix—O1—O2^x	135.54 (3)	O1ⁱⁱ—O3—O1^xiii	80.60 (2)
S—O1—O2^vii	112.24 (4)	O1^vii—O3—O1^xiii	87.80 (2)
Ni^vi—O1—O2^vii	78.20 (3)	O2^xiv—O3—O1^xiii	61.22 (2)
O2—O1—O2^vii	108.25 (3)	O2ⁱ—O3—O1^xiii	126.35 (2)
O1^v—O1—O2^vii	139.55 (3)	O2—O3—O1^xiii	101.16 (3)
O2^v—O1—O2^vii	80.89 (3)	O2^v—O3—O1^xiii	54.44 (2)
O2^vi—O1—O2^vii	117.27 (3)	Ni—O3—O1ⁱⁱⁱ	42.361 (14)
O3^vii—O1—O2^vii	58.80 (2)	Ni^v—O3—O1ⁱⁱⁱ	122.60 (3)
O2^viii—O1—O2^vii	45.69 (2)	O2^xiii—O3—O1ⁱⁱⁱ	144.99 (2)
O3^ix—O1—O2^vii	102.36 (3)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	49.402 (19)
O2^x—O1—O2^vii	81.85 (2)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	87.80 (2)
S—O1—O1^xi	89.28 (3)	O1^vii—O3—O1ⁱⁱⁱ	80.60 (2)
Ni^vi—O1—O1^xi	133.28 (4)	O2^xiv—O3—O1ⁱⁱⁱ	126.35 (2)
O2—O1—O1^xi	123.92 (4)	O2ⁱ—O3—O1ⁱⁱⁱ	61.22 (2)
O1^v—O1—O1^xi	80.57 (4)	O2—O3—O1ⁱⁱⁱ	54.44 (2)
O2^v—O1—O1^xi	65.47 (3)	O2^v—O3—O1ⁱⁱⁱ	101.16 (3)
O2^vi—O1—O1^xi	117.10 (4)	O1^xiii—O3—O1ⁱⁱⁱ	155.51 (4)
O3^vii—O1—O1^xi	85.53 (3)	Ni—O3—H	106.0 (14)
O2^viii—O1—O1^xi	120.84 (4)	Ni^v—O3—H	106.8 (14)
O3^ix—O1—O1^xi	177.46 (3)	O2^xiii—O3—H	118.8 (14)
O2^x—O1—O1^xi	43.19 (2)	O2ⁱⁱⁱ—O3—H	17.1 (14)
O2^vii—O1—O1^xi	75.49 (3)	O1ⁱⁱ—O3—H	146.7 (14)
S—O2—Ni	130.66 (4)	O1^vii—O3—H	74.5 (14)
S—O2—O1	35.48 (2)	O2^xiv—O3—H	71.0 (14)
Ni—O2—O1	160.26 (4)	O2ⁱ—O3—H	90.7 (14)
S—O2—O1^v	34.58 (2)	O2—O3—H	112.1 (14)
Ni—O2—O1^v	117.63 (3)	O2^v—O3—H	135.8 (14)
O1—O2—O1^v	59.92 (4)	O1^xiii—O3—H	131.1 (14)
S—O2—O2^v	35.43 (3)	O1ⁱⁱⁱ—O3—H	66.2 (14)
Ni—O2—O2^v	100.83 (2)	Ni—O3—H^v	106.8 (14)
O1—O2—O2^v	60.35 (3)	Ni^v—O3—H^v	106.0 (14)
O1^v—O2—O2^v	59.25 (2)	O2^xiii—O3—H^v	17.1 (14)
S—O2—O3^ix	106.85 (4)	O2ⁱⁱⁱ—O3—H^v	118.8 (14)
Ni—O2—O3^ix	122.31 (3)	O1ⁱⁱ—O3—H^v	74.5 (14)
O1—O2—O3^ix	72.71 (3)	O1^vii—O3—H^v	146.7 (14)
O1^v—O2—O3^ix	112.05 (4)	O2^xiv—O3—H^v	90.7 (14)
O2^v—O2—O3^ix	129.65 (4)	O2ⁱ—O3—H^v	71.0 (14)
S—O2—O1ⁱⁱⁱ	160.23 (4)	O2—O3—H^v	135.8 (14)
Ni—O2—O1ⁱⁱⁱ	47.45 (2)	O2^v—O3—H^v	112.1 (14)
O1—O2—O1ⁱⁱⁱ	137.96 (3)	O1^xiii—O3—H^v	66.2 (14)
O1^v—O2—O1ⁱⁱⁱ	161.84 (4)	O1ⁱⁱⁱ—O3—H^v	131.1 (14)
O2^v—O2—O1ⁱⁱⁱ	127.61 (2)	H—O3—H^v	107 (3)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x, −y+1, z−1/2; (v) −x, y, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) −x, −y, −z+1; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.820 (19)	1.904 (19)	2.6725 (8)	155.7 (19)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(NiSO4H2O_N2_273K) top

Crystal data top

H₂NiO₅S	V = 342.79 (9) Å³
M_r = 172.79	Z = 4
Monoclinic, C2/c	F(000) = 344
a = 6.8252 (10) Å	D_x = 3.348 Mg m⁻³
b = 7.607 (1) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.4587 (10) Å	µ = 6.15 mm⁻¹
β = 117.724 (10)°	T = 273 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.024
T_min = 0.637, T_max = 0.748	θ_max = 39.9°, θ_min = 4.3°
10744 measured reflections	h = −12→12
1064 independent reflections	k = −13→13
1031 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.015	w = 1/[σ²(F_o²) + (0.021P)² + 0.340P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.041	(Δ/σ)_max < 0.001
S = 1.13	Δρ_max = 0.67 e Å⁻³
1064 reflections	Δρ_min = −0.68 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0247 (13)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ni	0.000000	0.500000	0.000000	0.00577 (5)
S	0.000000	0.15681 (3)	0.250000	0.00527 (5)
O1	0.17279 (10)	0.04668 (9)	0.40353 (10)	0.01106 (10)
O2	0.10339 (10)	0.27006 (8)	0.15477 (9)	0.00926 (10)
O3	0.000000	0.63108 (12)	0.250000	0.00810 (12)
H	0.108 (3)	0.695 (2)	0.294 (3)	0.020 (4)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni	0.00521 (6)	0.00627 (7)	0.00552 (6)	−0.00020 (3)	0.00223 (4)	0.00023 (3)
S	0.00403 (9)	0.00542 (9)	0.00597 (9)	0.000	0.00201 (7)	0.000
O1	0.0065 (2)	0.0132 (3)	0.0125 (2)	0.00321 (18)	0.00356 (18)	0.00631 (19)
O2	0.0089 (2)	0.0086 (2)	0.0122 (2)	0.00120 (16)	0.00657 (18)	0.00377 (17)
O3	0.0076 (3)	0.0092 (3)	0.0076 (3)	0.000	0.0037 (2)	0.000

Geometric parameters (Å, º) top

Ni—O2	2.0328 (6)	O1—O1^iv	2.4047 (13)
Ni—O2ⁱ	2.0328 (6)	O1—O2^iv	2.4222 (9)
Ni—O1ⁱⁱ	2.0338 (7)	O1—O2^vi	2.7511 (9)
Ni—O1ⁱⁱⁱ	2.0338 (7)	O1—O3^vii	2.8503 (8)
Ni—O3ⁱ	2.1145 (5)	O1—O2^viii	2.9947 (10)
Ni—O3	2.1145 (5)	O1—O3^ix	3.0150 (7)
Ni—O2ⁱⁱⁱ	3.4195 (7)	O1—O2^x	3.2198 (10)
Ni—O2ⁱⁱ	3.4195 (7)	O1—O2^vii	3.2324 (11)
Ni—O2^iv	3.4465 (7)	O1—O1^xi	3.3610 (13)
Ni—O2^v	3.4465 (7)	O2—O2^iv	2.4238 (12)
S—O1	1.4654 (6)	O2—O3^ix	2.6760 (8)
S—O1^iv	1.4654 (6)	O2—O3ⁱ	2.8629 (8)
S—O2^iv	1.4869 (6)	O2—O3	3.0018 (11)
S—O2	1.4869 (6)	O3—H	0.813 (18)
O1—O2	2.3951 (9)	O3—H^iv	0.813 (18)

O2—Ni—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	77.09 (3)
O2—Ni—O1ⁱⁱ	94.85 (3)	S—O2—O3ⁱ	135.81 (4)
O2ⁱ—Ni—O1ⁱⁱ	85.15 (3)	Ni—O2—O3ⁱ	47.54 (2)
O2—Ni—O1ⁱⁱⁱ	85.15 (3)	O1—O2—O3ⁱ	150.02 (4)
O2ⁱ—Ni—O1ⁱⁱⁱ	94.85 (3)	O1^iv—O2—O3ⁱ	101.86 (3)
O1ⁱⁱ—Ni—O1ⁱⁱⁱ	180.0	O2^iv—O2—O3ⁱ	133.87 (4)
O2—Ni—O3ⁱ	87.28 (3)	O3^ix—O2—O3ⁱ	96.10 (2)
O2ⁱ—Ni—O3ⁱ	92.72 (3)	O1ⁱⁱⁱ—O2—O3ⁱ	60.99 (2)
O1ⁱⁱ—Ni—O3ⁱ	93.22 (2)	S—O2—O1ⁱⁱ	91.32 (3)
O1ⁱⁱⁱ—Ni—O3ⁱ	86.78 (2)	Ni—O2—O1ⁱⁱ	42.585 (17)
O2—Ni—O3	92.72 (3)	O1—O2—O1ⁱⁱ	126.72 (4)
O2ⁱ—Ni—O3	87.28 (3)	O1^iv—O2—O1ⁱⁱ	76.06 (3)
O1ⁱⁱ—Ni—O3	86.78 (2)	O2^iv—O2—O1ⁱⁱ	72.38 (3)
O1ⁱⁱⁱ—Ni—O3	93.22 (2)	O3^ix—O2—O1ⁱⁱ	157.99 (3)
O3ⁱ—Ni—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.03 (3)
O2—Ni—O2ⁱⁱⁱ	98.353 (14)	O3ⁱ—O2—O1ⁱⁱ	61.91 (2)
O2ⁱ—Ni—O2ⁱⁱⁱ	81.647 (14)	S—O2—O3	101.60 (3)
O1ⁱⁱ—Ni—O2ⁱⁱⁱ	136.52 (2)	Ni—O2—O3	44.719 (16)
O1ⁱⁱⁱ—Ni—O2ⁱⁱⁱ	43.48 (2)	O1—O2—O3	116.70 (3)
O3ⁱ—Ni—O2ⁱⁱⁱ	128.505 (16)	O1^iv—O2—O3	115.81 (3)
O3—Ni—O2ⁱⁱⁱ	51.495 (16)	O2^iv—O2—O3	66.189 (14)
O2—Ni—O2ⁱⁱ	81.648 (15)	O3^ix—O2—O3	128.23 (3)
O2ⁱ—Ni—O2ⁱⁱ	98.353 (15)	O1ⁱⁱⁱ—O2—O3	63.04 (2)
O1ⁱⁱ—Ni—O2ⁱⁱ	43.48 (2)	O3ⁱ—O2—O3	92.26 (2)
O1ⁱⁱⁱ—Ni—O2ⁱⁱ	136.52 (2)	O1ⁱⁱ—O2—O3	56.761 (17)
O3ⁱ—Ni—O2ⁱⁱ	51.495 (16)	S—O2—O1^xii	94.33 (3)
O3—Ni—O2ⁱⁱ	128.505 (16)	Ni—O2—O1^xii	114.81 (3)
O2ⁱⁱⁱ—Ni—O2ⁱⁱ	180.00 (2)	O1—O2—O1^xii	83.70 (2)
O2—Ni—O2^iv	43.67 (2)	O1^iv—O2—O1^xii	71.54 (3)
O2ⁱ—Ni—O2^iv	136.33 (2)	O2^iv—O2—O1^xii	128.65 (2)
O1ⁱⁱ—Ni—O2^iv	66.60 (2)	O3^ix—O2—O1^xii	56.93 (2)
O1ⁱⁱⁱ—Ni—O2^iv	113.40 (2)	O1ⁱⁱⁱ—O2—O1^xii	103.74 (3)
O3ⁱ—Ni—O2^iv	120.23 (2)	O3ⁱ—O2—O1^xii	67.27 (3)
O3—Ni—O2^iv	59.77 (2)	O1ⁱⁱ—O2—O1^xii	110.58 (3)
O2ⁱⁱⁱ—Ni—O2^iv	96.189 (18)	O3—O2—O1^xii	159.51 (3)
O2ⁱⁱ—Ni—O2^iv	83.811 (19)	S—O2—O1^vii	82.37 (3)
O2—Ni—O2^v	136.33 (2)	Ni—O2—O1^vii	94.72 (3)
O2ⁱ—Ni—O2^v	43.67 (2)	O1—O2—O1^vii	71.76 (3)
O1ⁱⁱ—Ni—O2^v	113.40 (2)	O1^iv—O2—O1^vii	116.42 (3)
O1ⁱⁱⁱ—Ni—O2^v	66.60 (2)	O2^iv—O2—O1^vii	62.01 (3)
O3ⁱ—Ni—O2^v	59.77 (2)	O3^ix—O2—O1^vii	87.70 (2)
O3—Ni—O2^v	120.23 (2)	O1ⁱⁱⁱ—O2—O1^vii	78.31 (2)
O2ⁱⁱⁱ—Ni—O2^v	83.811 (18)	O3ⁱ—O2—O1^vii	136.83 (3)
O2ⁱⁱ—Ni—O2^v	96.189 (19)	O1ⁱⁱ—O2—O1^vii	107.33 (3)
O2^iv—Ni—O2^v	180.000 (18)	O3—O2—O1^vii	54.262 (17)
O1—S—O1^iv	110.26 (6)	O1^xii—O2—O1^vii	142.02 (2)
O1—S—O2^iv	110.25 (4)	Ni—O3—Ni^iv	123.73 (4)
O1^iv—S—O2^iv	108.44 (3)	Ni—O3—O2ⁱⁱⁱ	90.308 (16)
O1—S—O2	108.44 (4)	Ni^iv—O3—O2ⁱⁱⁱ	111.545 (17)
O1^iv—S—O2	110.25 (4)	Ni—O3—O2^xiii	111.544 (17)
O2^iv—S—O2	109.19 (5)	Ni^iv—O3—O2^xiii	90.308 (16)
S—O1—Ni^vi	136.75 (4)	O2ⁱⁱⁱ—O3—O2^xiii	133.46 (4)
S—O1—O2	36.08 (2)	Ni—O3—O1ⁱⁱ	45.430 (17)
Ni^vi—O1—O2	100.77 (3)	Ni^iv—O3—O1ⁱⁱ	104.74 (3)
S—O1—O1^iv	34.87 (3)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	134.21 (2)
Ni^vi—O1—O1^iv	140.00 (5)	O2^xiii—O3—O1ⁱⁱ	71.19 (2)
O2—O1—O1^iv	60.61 (3)	Ni—O3—O1^vii	104.74 (3)
S—O1—O2^iv	35.16 (2)	Ni^iv—O3—O1^vii	45.430 (17)
Ni^vi—O1—O2^iv	145.16 (4)	O2ⁱⁱⁱ—O3—O1^vii	71.19 (2)
O2—O1—O2^iv	60.41 (3)	O2^xiii—O3—O1^vii	134.21 (2)
O1^iv—O1—O2^iv	59.50 (2)	O1ⁱⁱ—O3—O1^vii	123.36 (4)
S—O1—O2^vi	128.17 (4)	Ni—O3—O2^xiv	162.31 (3)
Ni^vi—O1—O2^vi	47.412 (19)	Ni^iv—O3—O2^xiv	45.174 (15)
O2—O1—O2^vi	110.15 (3)	O2ⁱⁱⁱ—O3—O2^xiv	83.90 (2)
O1^iv—O1—O2^vi	102.72 (3)	O2^xiii—O3—O2^xiv	84.19 (2)
O2^iv—O1—O2^vi	162.02 (4)	O1ⁱⁱ—O3—O2^xiv	141.77 (2)
S—O1—O3^vii	170.39 (4)	O1^vii—O3—O2^xiv	57.57 (2)
Ni^vi—O1—O3^vii	47.790 (15)	Ni—O3—O2ⁱ	45.174 (15)
O2—O1—O3^vii	145.90 (3)	Ni^iv—O3—O2ⁱ	162.31 (3)
O1^iv—O1—O3^vii	150.59 (2)	O2ⁱⁱⁱ—O3—O2ⁱ	84.19 (2)
O2^iv—O1—O3^vii	135.37 (3)	O2^xiii—O3—O2ⁱ	83.90 (2)
O2^vi—O1—O3^vii	61.44 (2)	O1ⁱⁱ—O3—O2ⁱ	57.57 (2)
S—O1—O2^viii	114.94 (4)	O1^vii—O3—O2ⁱ	141.77 (2)
Ni^vi—O1—O2^viii	42.560 (19)	O2^xiv—O3—O2ⁱ	149.54 (4)
O2—O1—O2^viii	86.41 (3)	Ni—O3—O2	42.565 (19)
O1^iv—O1—O2^viii	146.95 (3)	Ni^iv—O3—O2	82.74 (3)
O2^iv—O1—O2^viii	103.94 (3)	O2ⁱⁱⁱ—O3—O2	95.977 (17)
O2^vi—O1—O2^viii	89.97 (3)	O2^xiii—O3—O2	128.22 (3)
O3^vii—O1—O2^viii	61.75 (3)	O1ⁱⁱ—O3—O2	61.49 (2)
S—O1—O3^ix	92.89 (3)	O1^vii—O3—O2	67.00 (3)
Ni^vi—O1—O3^ix	44.445 (17)	O2^xiv—O3—O2	121.34 (3)
O2—O1—O3^ix	57.94 (2)	O2ⁱ—O3—O2	87.74 (2)
O1^iv—O1—O3^ix	102.12 (4)	Ni—O3—O2^iv	82.74 (3)
O2^iv—O1—O3^ix	115.75 (3)	Ni^iv—O3—O2^iv	42.565 (19)
O2^vi—O1—O3^ix	62.55 (3)	O2ⁱⁱⁱ—O3—O2^iv	128.22 (3)
O3^vii—O1—O3^ix	92.23 (2)	O2^xiii—O3—O2^iv	95.977 (17)
O2^viii—O1—O3^ix	56.90 (2)	O1ⁱⁱ—O3—O2^iv	67.00 (3)
S—O1—O2^x	126.85 (4)	O1^vii—O3—O2^iv	61.49 (2)
Ni^vi—O1—O2^x	95.63 (3)	O2^xiv—O3—O2^iv	87.74 (2)
O2—O1—O2^x	162.20 (4)	O2ⁱ—O3—O2^iv	121.34 (3)
O1^iv—O1—O2^x	102.10 (3)	O2—O3—O2^iv	47.62 (3)
O2^iv—O1—O2^x	108.45 (3)	Ni—O3—O1^xiii	122.57 (3)
O2^vi—O1—O2^x	76.26 (3)	Ni^iv—O3—O1^xiii	42.335 (14)
O3^vii—O1—O2^x	51.880 (19)	O2ⁱⁱⁱ—O3—O1^xiii	145.07 (2)
O2^viii—O1—O2^x	110.57 (3)	O2^xiii—O3—O1^xiii	49.337 (19)
O3^ix—O1—O2^x	135.72 (3)	O1ⁱⁱ—O3—O1^xiii	80.62 (2)
S—O1—O2^vii	112.14 (4)	O1^vii—O3—O1^xiii	87.77 (2)
Ni^vi—O1—O2^vii	78.12 (2)	O2^xiv—O3—O1^xiii	61.19 (2)
O2—O1—O2^vii	108.24 (3)	O2ⁱ—O3—O1^xiii	126.423 (19)
O1^iv—O1—O2^vii	139.45 (3)	O2—O3—O1^xiii	101.08 (3)
O2^iv—O1—O2^vii	80.78 (3)	O2^iv—O3—O1^xiii	54.42 (2)
O2^vi—O1—O2^vii	117.20 (3)	Ni—O3—O1ⁱⁱⁱ	42.335 (14)
O3^vii—O1—O2^vii	58.74 (2)	Ni^iv—O3—O1ⁱⁱⁱ	122.57 (3)
O2^viii—O1—O2^vii	45.62 (2)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	49.337 (19)
O3^ix—O1—O2^vii	102.29 (3)	O2^xiii—O3—O1ⁱⁱⁱ	145.07 (2)
O2^x—O1—O2^vii	81.795 (19)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	87.77 (2)
S—O1—O1^xi	89.16 (3)	O1^vii—O3—O1ⁱⁱⁱ	80.62 (2)
Ni^vi—O1—O1^xi	133.27 (4)	O2^xiv—O3—O1ⁱⁱⁱ	126.423 (19)
O2—O1—O1^xi	123.80 (4)	O2ⁱ—O3—O1ⁱⁱⁱ	61.19 (2)
O1^iv—O1—O1^xi	80.50 (3)	O2—O3—O1ⁱⁱⁱ	54.42 (2)
O2^iv—O1—O1^xi	65.33 (3)	O2^iv—O3—O1ⁱⁱⁱ	101.08 (3)
O2^vi—O1—O1^xi	117.25 (4)	O1^xiii—O3—O1ⁱⁱⁱ	155.41 (4)
O3^vii—O1—O1^xi	85.50 (3)	Ni—O3—H	105.6 (13)
O2^viii—O1—O1^xi	120.69 (4)	Ni^iv—O3—H	107.1 (13)
O3^ix—O1—O1^xi	177.37 (3)	O2ⁱⁱⁱ—O3—H	16.8 (13)
O2^x—O1—O1^xi	43.126 (19)	O2^xiii—O3—H	119.1 (13)
O2^vii—O1—O1^xi	75.39 (3)	O1ⁱⁱ—O3—H	146.3 (13)
S—O2—Ni	130.79 (4)	O1^vii—O3—H	74.5 (13)
S—O2—O1	35.48 (2)	O2^xiv—O3—H	71.4 (13)
Ni—O2—O1	160.34 (4)	O2ⁱ—O3—H	90.3 (13)
S—O2—O1^iv	34.58 (2)	O2—O3—H	111.9 (13)
Ni—O2—O1^iv	117.78 (3)	O2^iv—O3—H	135.8 (13)
O1—O2—O1^iv	59.89 (4)	O1^xiii—O3—H	131.6 (13)
S—O2—O2^iv	35.41 (3)	O1ⁱⁱⁱ—O3—H	65.8 (13)
Ni—O2—O2^iv	100.95 (2)	Ni—O3—H^iv	107.1 (13)
O1—O2—O2^iv	60.35 (3)	Ni^iv—O3—H^iv	105.6 (13)
O1^iv—O2—O2^iv	59.24 (2)	O2ⁱⁱⁱ—O3—H^iv	119.1 (13)
S—O2—O3^ix	106.89 (3)	O2^xiii—O3—H^iv	16.8 (13)
Ni—O2—O3^ix	122.12 (3)	O1ⁱⁱ—O3—H^iv	74.5 (13)
O1—O2—O3^ix	72.72 (3)	O1^vii—O3—H^iv	146.3 (13)
O1^iv—O2—O3^ix	112.16 (3)	O2^xiv—O3—H^iv	90.3 (13)
O2^iv—O2—O3^ix	129.59 (4)	O2ⁱ—O3—H^iv	71.4 (13)
S—O2—O1ⁱⁱⁱ	160.13 (4)	O2—O3—H^iv	135.8 (13)
Ni—O2—O1ⁱⁱⁱ	47.44 (2)	O2^iv—O3—H^iv	111.9 (13)
O1—O2—O1ⁱⁱⁱ	137.80 (3)	O1^xiii—O3—H^iv	65.8 (13)
O1^iv—O2—O1ⁱⁱⁱ	162.02 (4)	O1ⁱⁱⁱ—O3—H^iv	131.6 (13)
O2^iv—O2—O1ⁱⁱⁱ	127.60 (2)	H—O3—H^iv	107 (3)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x, y, −z+1/2; (v) x, −y+1, z−1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) −x, −y, −z+1; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.813 (18)	1.912 (18)	2.6760 (8)	156.1 (18)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

(NiSO4H2O_N2_313K) top

Crystal data top

H₂NiO₅S	V = 343.21 (9) Å³
M_r = 172.79	Z = 4
Monoclinic, C2/c	F(000) = 344
a = 6.8332 (10) Å	D_x = 3.344 Mg m⁻³
b = 7.6026 (10) Å	Mo Kα radiation, λ = 0.71073 Å
c = 7.4669 (10) Å	µ = 6.14 mm⁻¹
β = 117.776 (10)°	T = 313 K

Data collection top

Absorption correction: multi-scan SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10	R_int = 0.025
T_min = 0.630, T_max = 0.748	θ_max = 40.0°, θ_min = 4.3°
10700 measured reflections	h = −12→12
1068 independent reflections	k = −13→13
1034 reflections with I > 2σ(I)	l = −13→13

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.016	w = 1/[σ²(F_o²) + (0.021P)² + 0.330P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.042	(Δ/σ)_max < 0.001
S = 1.13	Δρ_max = 0.71 e Å⁻³
1068 reflections	Δρ_min = −0.61 e Å⁻³
40 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0267 (14)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ni	0.000000	0.500000	0.000000	0.00653 (5)
S	0.000000	0.15651 (3)	0.250000	0.00591 (5)
O1	0.17290 (10)	0.04625 (10)	0.40317 (10)	0.01253 (11)
O2	0.10276 (10)	0.26975 (8)	0.15448 (10)	0.01045 (10)
O3	0.000000	0.63132 (12)	0.250000	0.00908 (13)
H	0.107 (3)	0.696 (3)	0.294 (3)	0.023 (5)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni	0.00586 (6)	0.00709 (7)	0.00627 (6)	−0.00018 (4)	0.00251 (5)	0.00029 (3)
S	0.00440 (9)	0.00604 (9)	0.00675 (9)	0.000	0.00215 (7)	0.000
O1	0.0073 (2)	0.0148 (3)	0.0144 (2)	0.00359 (19)	0.00413 (19)	0.0072 (2)
O2	0.0100 (2)	0.0096 (2)	0.0141 (2)	0.00137 (17)	0.00752 (19)	0.00425 (17)
O3	0.0085 (3)	0.0103 (3)	0.0087 (3)	0.000	0.0043 (2)	0.000

Geometric parameters (Å, º) top

Ni—O2	2.0329 (6)	O1—O1^iv	2.4038 (13)
Ni—O2ⁱ	2.0329 (6)	O1—O2^iv	2.4217 (9)
Ni—O1ⁱⁱ	2.0338 (7)	O1—O2^vi	2.7512 (10)
Ni—O1ⁱⁱⁱ	2.0338 (7)	O1—O3^vii	2.8513 (8)
Ni—O3ⁱ	2.1169 (5)	O1—O2^viii	2.9948 (10)
Ni—O3	2.1169 (5)	O1—O3^ix	3.0174 (8)
Ni—O2ⁱⁱⁱ	3.4210 (7)	O1—O2^x	3.2188 (10)
Ni—O2ⁱⁱ	3.4210 (7)	O1—O2^vii	3.2399 (11)
Ni—O2^iv	3.4499 (7)	O1—O1^xi	3.3694 (14)
Ni—O2^v	3.4499 (7)	O2—O2^iv	2.4237 (13)
S—O1	1.4653 (7)	O2—O3^ix	2.6796 (8)
S—O1^iv	1.4654 (7)	O2—O3ⁱ	2.8642 (8)
S—O2	1.4865 (6)	O2—O3	3.0041 (11)
S—O2^iv	1.4865 (6)	O3—H	0.809 (19)
O1—O2	2.3949 (9)	O3—H^iv	0.809 (19)

O2—Ni—O2ⁱ	180.0	O3^ix—O2—O1ⁱⁱⁱ	76.85 (3)
O2—Ni—O1ⁱⁱ	94.85 (3)	S—O2—O3ⁱ	136.01 (4)
O2ⁱ—Ni—O1ⁱⁱ	85.15 (3)	Ni—O2—O3ⁱ	47.58 (2)
O2—Ni—O1ⁱⁱⁱ	85.15 (3)	O1—O2—O3ⁱ	150.00 (4)
O2ⁱ—Ni—O1ⁱⁱⁱ	94.85 (3)	O1^iv—O2—O3ⁱ	102.04 (3)
O1ⁱⁱ—Ni—O1ⁱⁱⁱ	180.00 (4)	O2^iv—O2—O3ⁱ	134.11 (4)
O2—Ni—O3ⁱ	87.27 (3)	O3^ix—O2—O3ⁱ	95.97 (2)
O2ⁱ—Ni—O3ⁱ	92.73 (3)	O1ⁱⁱⁱ—O2—O3ⁱ	60.99 (2)
O1ⁱⁱ—Ni—O3ⁱ	93.25 (2)	S—O2—O1ⁱⁱ	91.52 (3)
O1ⁱⁱⁱ—Ni—O3ⁱ	86.75 (2)	Ni—O2—O1ⁱⁱ	42.583 (18)
O2—Ni—O3	92.73 (3)	O1—O2—O1ⁱⁱ	126.92 (4)
O2ⁱ—Ni—O3	87.27 (3)	O1^iv—O2—O1ⁱⁱ	76.22 (3)
O1ⁱⁱ—Ni—O3	86.75 (2)	O2^iv—O2—O1ⁱⁱ	72.58 (3)
O1ⁱⁱⁱ—Ni—O3	93.25 (2)	O3^ix—O2—O1ⁱⁱ	157.88 (3)
O3ⁱ—Ni—O3	180.0	O1ⁱⁱⁱ—O2—O1ⁱⁱ	90.02 (3)
O2—Ni—O2ⁱⁱⁱ	98.361 (14)	O3ⁱ—O2—O1ⁱⁱ	61.95 (2)
O2ⁱ—Ni—O2ⁱⁱⁱ	81.638 (15)	S—O2—O3	101.60 (3)
O1ⁱⁱ—Ni—O2ⁱⁱⁱ	136.56 (2)	Ni—O2—O3	44.739 (16)
O1ⁱⁱⁱ—Ni—O2ⁱⁱⁱ	43.44 (2)	O1—O2—O3	116.72 (3)
O3ⁱ—Ni—O2ⁱⁱⁱ	128.439 (16)	O1^iv—O2—O3	115.83 (3)
O3—Ni—O2ⁱⁱⁱ	51.561 (16)	O2^iv—O2—O3	66.210 (14)
O2—Ni—O2ⁱⁱ	81.639 (15)	O3^ix—O2—O3	128.03 (3)
O2ⁱ—Ni—O2ⁱⁱ	98.361 (15)	O1ⁱⁱⁱ—O2—O3	63.06 (2)
O1ⁱⁱ—Ni—O2ⁱⁱ	43.44 (2)	O3ⁱ—O2—O3	92.32 (2)
O1ⁱⁱⁱ—Ni—O2ⁱⁱ	136.56 (2)	O1ⁱⁱ—O2—O3	56.758 (18)
O3ⁱ—Ni—O2ⁱⁱ	51.561 (16)	S—O2—O1^xii	94.55 (3)
O3—Ni—O2ⁱⁱ	128.439 (16)	Ni—O2—O1^xii	114.69 (3)
O2ⁱⁱⁱ—Ni—O2ⁱⁱ	180.0	O1—O2—O1^xii	83.81 (2)
O2—Ni—O2^iv	43.58 (2)	O1^iv—O2—O1^xii	71.79 (3)
O2ⁱ—Ni—O2^iv	136.42 (2)	O2^iv—O2—O1^xii	128.88 (2)
O1ⁱⁱ—Ni—O2^iv	66.74 (3)	O3^ix—O2—O1^xii	56.94 (2)
O1ⁱⁱⁱ—Ni—O2^iv	113.26 (3)	O1ⁱⁱⁱ—O2—O1^xii	103.52 (3)
O3ⁱ—Ni—O2^iv	120.25 (2)	O3ⁱ—O2—O1^xii	67.12 (3)
O3—Ni—O2^iv	59.75 (3)	O1ⁱⁱ—O2—O1^xii	110.63 (3)
O2ⁱⁱⁱ—Ni—O2^iv	96.124 (19)	O3—O2—O1^xii	159.41 (3)
O2ⁱⁱ—Ni—O2^iv	83.876 (19)	S—O2—O1^vii	82.29 (3)
O2—Ni—O2^v	136.42 (2)	Ni—O2—O1^vii	94.64 (3)
O2ⁱ—Ni—O2^v	43.58 (2)	O1—O2—O1^vii	71.77 (3)
O1ⁱⁱ—Ni—O2^v	113.26 (3)	O1^iv—O2—O1^vii	116.33 (3)
O1ⁱⁱⁱ—Ni—O2^v	66.74 (3)	O2^iv—O2—O1^vii	61.88 (3)
O3ⁱ—Ni—O2^v	59.75 (3)	O3^ix—O2—O1^vii	87.64 (2)
O3—Ni—O2^v	120.25 (3)	O1ⁱⁱⁱ—O2—O1^vii	78.24 (2)
O2ⁱⁱⁱ—Ni—O2^v	83.876 (19)	O3ⁱ—O2—O1^vii	136.77 (3)
O2ⁱⁱ—Ni—O2^v	96.124 (19)	O1ⁱⁱ—O2—O1^vii	107.28 (3)
O2^iv—Ni—O2^v	180.000 (18)	O3—O2—O1^vii	54.182 (17)
O1—S—O1^iv	110.21 (6)	O1^xii—O2—O1^vii	142.03 (3)
O1—S—O2	108.45 (4)	Ni—O3—Ni^iv	123.72 (4)
O1^iv—S—O2	110.25 (4)	Ni—O3—O2^xiii	111.518 (18)
O1—S—O2^iv	110.25 (4)	Ni^iv—O3—O2^xiii	90.210 (15)
O1^iv—S—O2^iv	108.45 (4)	Ni—O3—O2ⁱⁱⁱ	90.210 (16)
O2—S—O2^iv	109.22 (5)	Ni^iv—O3—O2ⁱⁱⁱ	111.519 (18)
S—O1—Ni^vi	136.82 (4)	O2^xiii—O3—O2ⁱⁱⁱ	133.75 (5)
S—O1—O2	36.07 (2)	Ni—O3—O1ⁱⁱ	45.408 (17)
Ni^vi—O1—O2	100.84 (3)	Ni^iv—O3—O1ⁱⁱ	104.80 (3)
S—O1—O1^iv	34.89 (3)	O2^xiii—O3—O1ⁱⁱ	71.10 (2)
Ni^vi—O1—O1^iv	140.21 (5)	O2ⁱⁱⁱ—O3—O1ⁱⁱ	134.09 (2)
O2—O1—O1^iv	60.62 (3)	Ni—O3—O1^vii	104.80 (3)
S—O1—O2^iv	35.16 (2)	Ni^iv—O3—O1^vii	45.408 (17)
Ni^vi—O1—O2^iv	145.03 (4)	O2^xiii—O3—O1^vii	134.09 (2)
O2—O1—O2^iv	60.42 (3)	O2ⁱⁱⁱ—O3—O1^vii	71.10 (2)
O1^iv—O1—O2^iv	59.51 (3)	O1ⁱⁱ—O3—O1^vii	123.48 (5)
S—O1—O2^vi	128.34 (4)	Ni—O3—O2^xiv	162.35 (3)
Ni^vi—O1—O2^vi	47.41 (2)	Ni^iv—O3—O2^xiv	45.151 (16)
O2—O1—O2^vi	110.21 (3)	O2^xiii—O3—O2^xiv	84.13 (2)
O1^iv—O1—O2^vi	102.91 (3)	O2ⁱⁱⁱ—O3—O2^xiv	84.03 (2)
O2^iv—O1—O2^vi	162.22 (4)	O1ⁱⁱ—O3—O2^xiv	141.74 (2)
S—O1—O3^vii	170.20 (5)	O1^vii—O3—O2^xiv	57.55 (2)
Ni^vi—O1—O3^vii	47.838 (16)	Ni—O3—O2ⁱ	45.151 (16)
O2—O1—O3^vii	146.00 (3)	Ni^iv—O3—O2ⁱ	162.35 (3)
O1^iv—O1—O3^vii	150.60 (2)	O2^xiii—O3—O2ⁱ	84.03 (2)
O2^iv—O1—O3^vii	135.17 (4)	O2ⁱⁱⁱ—O3—O2ⁱ	84.13 (2)
O2^vi—O1—O3^vii	61.46 (2)	O1ⁱⁱ—O3—O2ⁱ	57.55 (2)
S—O1—O2^viii	114.86 (4)	O1^vii—O3—O2ⁱ	141.74 (2)
Ni^vi—O1—O2^viii	42.563 (19)	O2^xiv—O3—O2ⁱ	149.55 (4)
O2—O1—O2^viii	86.44 (3)	Ni—O3—O2	42.528 (19)
O1^iv—O1—O2^viii	146.97 (3)	Ni^iv—O3—O2	82.75 (3)
O2^iv—O1—O2^viii	103.78 (3)	O2^xiii—O3—O2	128.03 (3)
O2^vi—O1—O2^viii	89.98 (3)	O2ⁱⁱⁱ—O3—O2	95.896 (17)
O3^vii—O1—O2^viii	61.79 (3)	O1ⁱⁱ—O3—O2	61.46 (2)
S—O1—O3^ix	92.97 (3)	O1^vii—O3—O2	67.13 (3)
Ni^vi—O1—O3^ix	44.462 (17)	O2^xiv—O3—O2	121.40 (3)
O2—O1—O3^ix	57.99 (2)	O2ⁱ—O3—O2	87.68 (2)
O1^iv—O1—O3^ix	102.27 (4)	Ni—O3—O2^iv	82.75 (3)
O2^iv—O1—O3^ix	115.75 (3)	Ni^iv—O3—O2^iv	42.528 (19)
O2^vi—O1—O3^ix	62.57 (3)	O2^xiii—O3—O2^iv	95.896 (17)
O3^vii—O1—O3^ix	92.30 (2)	O2ⁱⁱⁱ—O3—O2^iv	128.03 (3)
O2^viii—O1—O3^ix	56.90 (2)	O1ⁱⁱ—O3—O2^iv	67.13 (3)
S—O1—O2^x	126.66 (4)	O1^vii—O3—O2^iv	61.46 (2)
Ni^vi—O1—O2^x	95.81 (3)	O2^xiv—O3—O2^iv	87.68 (2)
O2—O1—O2^x	162.03 (4)	O2ⁱ—O3—O2^iv	121.40 (3)
O1^iv—O1—O2^x	101.97 (3)	O2—O3—O2^iv	47.58 (3)
O2^iv—O1—O2^x	108.21 (3)	Ni—O3—O1^xiii	122.52 (3)
O2^vi—O1—O2^x	76.48 (3)	Ni^iv—O3—O1^xiii	42.292 (14)
O3^vii—O1—O2^x	51.96 (2)	O2^xiii—O3—O1^xiii	49.281 (19)
O2^viii—O1—O2^x	110.63 (3)	O2ⁱⁱⁱ—O3—O1^xiii	145.16 (2)
O3^ix—O1—O2^x	135.95 (3)	O1ⁱⁱ—O3—O1^xiii	80.63 (2)
S—O1—O2^vii	112.03 (4)	O1^vii—O3—O1^xiii	87.70 (2)
Ni^vi—O1—O2^vii	78.04 (3)	O2^xiv—O3—O1^xiii	61.15 (2)
O2—O1—O2^vii	108.23 (3)	O2ⁱ—O3—O1^xiii	126.52 (2)
O1^iv—O1—O2^vii	139.32 (3)	O2—O3—O1^xiii	100.97 (3)
O2^iv—O1—O2^vii	80.65 (3)	O2^iv—O3—O1^xiii	54.37 (2)
O2^vi—O1—O2^vii	117.13 (3)	Ni—O3—O1ⁱⁱⁱ	42.292 (14)
O3^vii—O1—O2^vii	58.69 (2)	Ni^iv—O3—O1ⁱⁱⁱ	122.52 (3)
O2^viii—O1—O2^vii	45.54 (2)	O2^xiii—O3—O1ⁱⁱⁱ	145.16 (2)
O3^ix—O1—O2^vii	102.22 (3)	O2ⁱⁱⁱ—O3—O1ⁱⁱⁱ	49.280 (19)
O2^x—O1—O2^vii	81.73 (2)	O1ⁱⁱ—O3—O1ⁱⁱⁱ	87.70 (2)
S—O1—O1^xi	89.01 (3)	O1^vii—O3—O1ⁱⁱⁱ	80.63 (2)
Ni^vi—O1—O1^xi	133.29 (4)	O2^xiv—O3—O1ⁱⁱⁱ	126.52 (2)
O2—O1—O1^xi	123.63 (4)	O2ⁱ—O3—O1ⁱⁱⁱ	61.15 (2)
O1^iv—O1—O1^xi	80.41 (4)	O2—O3—O1ⁱⁱⁱ	54.37 (2)
O2^iv—O1—O1^xi	65.15 (3)	O2^iv—O3—O1ⁱⁱⁱ	100.97 (3)
O2^vi—O1—O1^xi	117.45 (4)	O1^xiii—O3—O1ⁱⁱⁱ	155.25 (4)
O3^vii—O1—O1^xi	85.47 (3)	Ni—O3—H	105.8 (14)
O2^viii—O1—O1^xi	120.52 (4)	Ni^iv—O3—H	107.3 (13)
O3^ix—O1—O1^xi	177.28 (4)	O2^xiii—O3—H	118.6 (13)
O2^x—O1—O1^xi	43.06 (2)	O2ⁱⁱⁱ—O3—H	17.4 (13)
O2^vii—O1—O1^xi	75.28 (3)	O1ⁱⁱ—O3—H	146.2 (14)
S—O2—Ni	130.95 (4)	O1^vii—O3—H	75.1 (13)
S—O2—O1	35.48 (2)	O2^xiv—O3—H	71.4 (14)
Ni—O2—O1	160.43 (4)	O2ⁱ—O3—H	90.0 (14)
S—O2—O1^iv	34.59 (2)	O2—O3—H	112.6 (13)
Ni—O2—O1^iv	117.96 (3)	O2^iv—O3—H	136.3 (13)
O1—O2—O1^iv	59.87 (4)	O1^xiii—O3—H	131.4 (14)
S—O2—O2^iv	35.39 (3)	O1ⁱⁱⁱ—O3—H	66.3 (14)
Ni—O2—O2^iv	101.09 (2)	Ni—O3—H^iv	107.3 (13)
O1—O2—O2^iv	60.34 (3)	Ni^iv—O3—H^iv	105.8 (14)
O1^iv—O2—O2^iv	59.24 (3)	O2^xiii—O3—H^iv	17.4 (14)
S—O2—O3^ix	106.93 (4)	O2ⁱⁱⁱ—O3—H^iv	118.6 (13)
Ni—O2—O3^ix	121.90 (3)	O1ⁱⁱ—O3—H^iv	75.1 (13)
O1—O2—O3^ix	72.73 (3)	O1^vii—O3—H^iv	146.2 (14)
O1^iv—O2—O3^ix	112.29 (4)	O2^xiv—O3—H^iv	90.0 (14)
O2^iv—O2—O3^ix	129.52 (4)	O2ⁱ—O3—H^iv	71.4 (14)
S—O2—O1ⁱⁱⁱ	160.02 (4)	O2—O3—H^iv	136.3 (13)
Ni—O2—O1ⁱⁱⁱ	47.44 (2)	O2^iv—O3—H^iv	112.6 (13)
O1—O2—O1ⁱⁱⁱ	137.62 (3)	O1^xiii—O3—H^iv	66.3 (14)
O1^iv—O2—O1ⁱⁱⁱ	162.22 (4)	O1ⁱⁱⁱ—O3—H^iv	131.4 (14)
O2^iv—O2—O1ⁱⁱⁱ	127.59 (2)	H—O3—H^iv	105 (3)

Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, −y+1/2, z−1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x, y, −z+1/2; (v) x, −y+1, z−1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, y−1/2, z; (x) x, −y, z+1/2; (xi) −x, −y, −z+1; (xii) x, −y, z−1/2; (xiii) x−1/2, y+1/2, z; (xiv) x, −y+1, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H···O2ⁱⁱⁱ	0.809 (19)	1.923 (18)	2.6796 (8)	155.3 (19)

Symmetry code: (iii) −x+1/2, y+1/2, −z+1/2.

Acknowledgements

Technical assistance by G. Giester (Vienna) with the ℓ-N₂ data collections (313–113 K, Apex II diffractometer) and by A. F. Achkasov (Novosibirsk) with the ℓ-He data collections (75–15 K, Gemini R Ultra diffractometer) is gratefully acknowledged. The equipment of the Research and Education Center `Molecular design and ecologically safe technologies' (Novosibirsk State University) was used for the experiments. Constructive reviews by three anonymous referees are greatly appreciated.

Funding information

This work was supported by a grant from the Austrian Science Fund (FWF) (grant No. P 29149-N29), and the Russian Ministry of Science and Higher Education (grant No. AAAA-A21-121011390011-4 awarded to EVB, ZBA and NEB).

References

Alboom, A. V., De Resende, V. G., De Grave, E. & Gómez, J. A. M. (2009). J. Mol. Struct. 924–926, 448–456. Web of Science CrossRef Google Scholar
Anderson, O. L. (1995). Equations of State of Solids for Geophysics and Ceramic Science. Oxford University Press. Google Scholar
Angel, R. J., Gonzalez-Platas, J. & Alvaro, M. (2014). Z. Kristallogr. 229, 405–419. Web of Science CrossRef CAS Google Scholar
Arvidson, R. E., Poulet, F., Bibring, J.-P., Wolff, M., Gendrin, A., Morris, R. V., Freeman, J. J., Langevin, Y., Mangold, N. & Bellucci, G. (2005). Science, 307, 1591–1594. Web of Science CrossRef PubMed CAS Google Scholar
Ashkenazy, Y. (2019). Heliyon, 5, e01908. Web of Science CrossRef PubMed Google Scholar
Bao, X., He, M., Zhang, Z. & Liu, X. (2021). Crystals, 11, 14. Web of Science CrossRef Google Scholar
Bechtold, A. & Wildner, M. (2016). Eur. J. Mineral. 28, 43–52. Web of Science CrossRef CAS Google Scholar
Bishop, J. L., Darby Dyar, M., Lane, M. D. & Banfield, L. F. (2004). Int. J. Astrobiology, 3, 275–285. CrossRef CAS Google Scholar
Bishop, J. L., Parente, M., Weitz, C. M., Noe Dobrea, E. Z., Roach, L. H., Murchie, S. L., McGuire, P. C., McKeown, N. K., Rossi, C. M., Brown, A. J., Calvin, W. M., Milliken, R. & Mustard, J. F. (2009). J. Geophys. Res. 114, E00D09. Google Scholar
Brand, H. E. A., Fortes, A. D., Wood, I. G., Knight, K. S. & Vočadlo, L. (2009). Phys. Chem. Miner. 36, 29–46. Web of Science CrossRef ICSD CAS Google Scholar
Bruker (2012). APEX2 V1.0. and SADABS 2012/1, Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Burgess, R., Wright, I. P. & Pillinger, P. T. (1991). Meteoritics, 26, 55–64. CrossRef CAS Web of Science Google Scholar
Cardell, C., Sánchez-Navas, A., Olmo-Reyes, F. J. & Martín-Ramos, J. D. (2007). Anal. Chem. 79, 4455–4462. Web of Science CrossRef PubMed CAS Google Scholar
Chipera, S. J. & Vaniman, D. T. (2007). Geochim. Cosmochim. Acta, 71, 241–250. Web of Science CrossRef CAS Google Scholar
Chipera, S. J., Vaniman, D. T. & Carey, J. W. (2006). Proceedings of the 37th Annual Lunar and Planetary Science Conference (LPSC06), 13–17 March 2006, League City, TX, USA. Abstract 1457. Google Scholar
Christensen, P. R., Wyatt, M. B., Glotch, T. D., Rogers, A. D., Anwar, S., Arvidson, R. E., Bandfield, J. L., Blaney, D. L., Budney, C., Calvin, W. M., Fallacaro, A., Fergason, R. L., Gorelick, N., Graff, T. G., Hamilton, V. E., Hayes, A. G., Johnson, J. R., Knudson, A. T., McSween, H. Y. Jr, Mehall, G. L., Mehall, L. K., Moersch, J. E., Morris, R. V., Smith, M. D., Squyres, S. W., Ruff, S. W. & Wolff, M. J. (2004). Science, 306, 1733–1739. Web of Science CrossRef PubMed CAS Google Scholar
Clark, B. C. & Van Hart, D. C. (1981). Icarus, 45, 370–378. CrossRef CAS Web of Science Google Scholar
Clark, B. C., Morris, R. V., McLennan, S. M., Gellert, R., Jolliff, B., Knoll, A. H., Squyres, S. W., Lowenstein, T. K., Ming, D. W., Tosca, N. J., Yen, A., Christensen, P. R., Gorevan, S., Brückner, J., Calvin, W., Dreibus, G., Farrand, W., Klingelhoefer, G., Waenke, H., Zipfel, J., Bell, J. F. III, Grotzinger, J., McSween, H. Y. & Rieder, R. (2005). Earth Planet. Sci. Lett. 240, 73–94. Web of Science CrossRef CAS Google Scholar
Cloutis, E. A., Craig, M. A., Mustard, J. F., Kruzelecky, R. V., Jamroz, W. R., Scott, A., Bish, D. L., Poulet, F., Bibring, J.-P. & King, P. L. (2007). Geophys. Res. Lett. 34, L20202. Web of Science CrossRef Google Scholar
Combe, J.-P., Le Mouélic, S., Sotin, C., Gendrin, A., Mustard, J. F., Le Deit, L., Launeau, P., Bibring, J.-P., Gondet, B., Langevin, Y. & Pinet, P. (2008). Planet. Space Sci. 56, 951–975. Web of Science CrossRef CAS Google Scholar
Dalton, J. B., Prieto-Ballesteros, O., Kargel, J. S., Jamieson, C. S., Jolivet, J. & Quinn, R. (2005). Icarus, 177, 472–490. Web of Science CrossRef CAS Google Scholar
Dalton, J. B., Shirley, J. H. & Kamp, L. W. (2012). J. Geophys. Res. 117, E03003. Google Scholar
Deffrennes, G., Gardiola, B., Jeanneau, E., Mikaelian, G., Benigni, P., Pasturel, A., Pisch, A., Andrieux, J. & Dezellus, O. (2019). J. Solid State Chem. 273, 150–157. Web of Science CrossRef ICSD CAS Google Scholar
Dinsdale, A., Fang, C., Que, Z. & Fan, Z. (2019). JOM, 71, 1731–1736. Web of Science CrossRef CAS Google Scholar
Downs, R. T., Gibbs, G. V., Bartelmehs, K. L. & Boisen, M. B. (1992). Am. Mineral. 77, 751–757. CAS Google Scholar
Drebushchak, V. A. (2020). J. Therm. Anal. Calorim. 142, 1097–1113. Web of Science CrossRef CAS Google Scholar
Ende, M., Kirkkala, T., Loitzenbauer, M., Talla, D., Wildner, M. & Miletich, R. (2020). Inorg. Chem. 59, 6255–6266. Web of Science CrossRef ICSD CAS PubMed Google Scholar
Evans, H. T. Jr (1979). Phys. Chem. Miner. 4, 77–82. CrossRef CAS Web of Science Google Scholar
Fei, V. (1995). Thermal expansion. In Mineral Physics & Crystallography: a Handbook of Physical Constants, edited by T. J. Ahrens. Washington DC: American Geophysical Union. Google Scholar
Fortes, A. D., Fernandez-Alonso, F., Tucker, M. & Wood, I. G. (2017a). Acta Cryst. B73, 33–46. Web of Science CrossRef IUCr Journals Google Scholar
Fortes, A. D., Knight, K. S. & Wood, I. G. (2017b). Acta Cryst. B73, 47–64. Web of Science CrossRef IUCr Journals Google Scholar
Fortes, A. D., Wood, I. G., Alfredsson, M., Vočadlo, L. & Knight, K. S. (2006). Eur. J. Mineral. 18, 449–462. Web of Science CrossRef CAS Google Scholar
Fortes, A. D., Wood, I. G. & Knight, K. S. (2008). Phys. Chem. Miner. 35, 207–221. Web of Science CrossRef ICSD CAS Google Scholar
Fortes, A. D., Wood, I. G., Vočadlo, L., Brand, H. E. A. & Knight, K. S. (2007). J. Appl. Cryst. 40, 761–770. Web of Science CrossRef CAS IUCr Journals Google Scholar
Fredriksson, K. & Kerridge, J. F. (1988). Meteoritics, 23, 35–44. CrossRef PubMed CAS Web of Science Google Scholar
Gonzalez-Platas, J., Alvaro, M., Nestola, F. & Angel, R. (2016). J. Appl. Cryst. 49, 1377–1382. Web of Science CrossRef CAS IUCr Journals Google Scholar
Hawthorne, F. C., Groat, L. A., Raudsepp, M. & Ercit, T. S. (1987). N. Jahrb. Min. Abh. 157, 121–132. CAS Google Scholar
Hazen, R. M., Downs, R. T. & Prewitt, C. T. (2000). Rev. Min. Geochem. 41, 2–33. CrossRef Google Scholar
Hazen, R. M. & Finger, L. W. (1982a). Comparative Crystal Chemistry. New York: Wiley. Google Scholar
Hazen, R. M. & Finger, L. W. (1982b). High-temperature and High-Pressure Crystal Chemistry. In High-Pressure Researches in Geoscience, edited by W. Schreyer W. Stuttgart: Schweizerbart. Google Scholar
Hazen, R. M. & Prewitt, C. T. (1977). Am. Mineral. 62, 309–315. CAS Google Scholar
Jamieson, C. S., Noe Dobrea, E. Z., Dalton, J. B. III, Pitman, K. M. & Abbey, W. Z. (2014). J. Geophys. Res. Planets, 119, 1218–1237. Web of Science CrossRef CAS Google Scholar
Kaminski, W. (2014). WinTensor.https://cad4.cpac.washington.edu/WinTensorhome/WinTensor.htm. Google Scholar
Kargel, J. S. (1991). Icarus, 94, 368–390. CrossRef CAS Web of Science Google Scholar
Keil, K., Clark, B. C., Baird, A. K., Toulmin, P. III & Rose, H. J. J. (1978). Naturwissenschaften, 65, 231–238. CrossRef CAS Web of Science Google Scholar
King, H. E. & Finger, L. W. (1979). J. Appl. Cryst. 12, 374–378. CrossRef CAS IUCr Journals Web of Science Google Scholar
McCord, T. B., Hansen, G. B. & Hibbitts, C. A. (2001a). Science, 292, 1523–1525. Web of Science CrossRef PubMed CAS Google Scholar
McCord, T. B., Orlando, T. M., Teeter, G., Hansen, G. B., Sieger, M. T., Petrik, N. G. & Van Keulen, L. (2001b). J. Geophys. Res. 106, 3311–3319. Web of Science CrossRef CAS Google Scholar
Meusburger, J. M., Ende, M., Matzinger, P., Talla, D., Miletich, R. & Wildner, M. (2020). Icarus, 336, 113459. Web of Science CrossRef Google Scholar
Meusburger, J. M., Ende, M., Talla, D., Wildner, M. & Miletich, R. (2019). J. Solid State Chem. 277, 240–252. Web of Science CrossRef ICSD CAS Google Scholar
Momma, K. & Izumi, F. (2011). J. Appl. Cryst. 44, 1272–1276. Web of Science CrossRef CAS IUCr Journals Google Scholar
Nakamura, R. & Ohtani, E. (2011). Icarus, 211, 648–654. Web of Science CrossRef CAS Google Scholar
Papike, J. J., Burger, P. V., Karner, J. M. & Shearer, C. K. (2007). Proceedings of the 7th International Conference on Mars, 9 July 2007, Albuquerque, New Mexico, USA. Abstract 87131. Google Scholar
Peterson, R. C. & Wang, R. (2006). Geol, 34, 957–960. Web of Science CrossRef CAS Google Scholar
Poch, O., Istiqomah, I., Quirico, E., Beck, P., Schmitt, B., Theulé, P., Faure, A., Hilly Blant, P., Bonal, L., Raponi, A., Ciarniello, M., Rousseau, B., Potin, S., Brissaud, O., Flandinet, L., Filacchione, G., Pommerol, A., Thomas, N., Kappel, D., Mennella, V., Moroz, L., Vinogradoff, V., Arnold, G., Erard, S., Bockelée-Morvan, D., Leyrat, C., Capaccioni, F., De Sanctis, M. C., Longobardo, A., Mancarella, F., Palomba, E. & Tosi, F. (2020). Science, 367, eaaw7462. Web of Science CrossRef PubMed Google Scholar
Richardson, S. M. (1978). Meteoritics, 13, 141–159. CrossRef CAS Google Scholar
Rigaku Oxford Diffraction (2016). CrysAlis PRO. Rigaku Oxford Diffraction, The Woodlands, Texas, USA. Google Scholar
Schofield, P. F. & Knight, K. S. (2000). Physica B, 276–278, 897–898. Web of Science CrossRef CAS Google Scholar
Schofield, P. F., Knight, K. S. & Stretton, I. C. (1996). Am. Mineral. 81, 847–851. CrossRef CAS Google Scholar
Sekine, Y., Shibuya, T., Postberg, F., Hsu, H.-W., Suzuki, K., Masaki, Y., Kuwatani, T., Mori, M., Hong, P. K., Yoshizaki, M., Tachibana, S. & Sirono, S. (2015). Nat. Commun. 6, 8604. Web of Science CrossRef PubMed Google Scholar
Sharp, Z. D., Hazen, R. M. & Finger, L. W. (1987). Am. Mineral. 72, 748–755. CAS Google Scholar
Sheldrick, G. M. (2015). Acta Cryst. C71, 3–8. Web of Science CrossRef IUCr Journals Google Scholar
Solomonidou, A., Coustenis, A., Bampasidis, G., Kyriakopoulos, K., Moussas, X., Bratsolis, E. & Hirtzig, M. (2011). J. Cosmol. 13, 4191–4211. Google Scholar
Talla, D., Balla, M., Aicher, C., Lengauer, C. L. & Wildner, M. (2020). Am. Mineral. 105, 1472–1489. Web of Science CrossRef Google Scholar
Talla, D. & Wildner, M. (2019). Am. Mineral. 104, 1732–1749. Web of Science CrossRef Google Scholar
Tani, A., Hasegawa, N., Norizawa, K., Yada, T. & Ikeya, M. (2012). Radiat. Meas. 47, 890–893. Web of Science CrossRef CAS Google Scholar
Wang, A., Freeman, J. J. & Jolliff, B. L. (2009). J. Geophys. Res. 114, E04010. Google Scholar
Wildner, M., Ende, M., Meusburger, J. M., Kunit, R., Matzinger, P., Talla, D. & Miletich, R. (2021). Z. Kristallogr. 236, 225–237. Web of Science CrossRef ICSD Google Scholar
Wildner, M. & Giester, G. (1991). N. Jahrb. Min. Monatsh. 1991, 296–306. Google Scholar
Wilson, S. A. & Bish, D. L. (2012). Geochim. Cosmochim. Acta, 96, 120–133. Web of Science CrossRef CAS Google Scholar
Witzke, A., Arnold, G. & Stöffler, D. (2007). Planet. Space Sci. 55, 429–440. Web of Science CrossRef CAS Google Scholar
Zakharov, B. A., Miletich, R., Bogdanov, N. E. & Boldyreva, E. V. (2021). J. Appl. Cryst. 54, 1271–1275. Web of Science CrossRef CAS IUCr Journals Google Scholar

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Volume 9| Part 2| March 2022| Pages 194-203

ISSN: 2052-2525

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