High-pressure preference for reduced water content in porous zinc aspartate hydrates

The zinc aspartate (ZnAsp₂) complex, a common dietary supplement, preferentially crystallizes as the dihydrate (ZnAsp₂·2H₂O) from aqueous solution. Under normal conditions the dihydrate easily transforms into the sesquihydrate (ZnAsp₂·1.5H₂O). The dihydrate crystal structure is triclinic, space group P1, and the sesquihydrate is monoclinic, space group C2/c. However, their structures are closely related and similarly consist of zinc aspartate ribbons parallel to pores accommodating water molecules. These porous structures can breathe water molecules in and out depending on the temperature and air humidity. High pressure above 50 MPa favours the sesquihydrate, as shown by recrystallizations under pressure and compressibility measured by single-crystal X-ray diffraction up to 4 GPa. This preference is explained by the reduced volume of the sesquihydrate and water compressed separately, compared with the dihydrate. The sesquihydrate undergoes an isostructural phase transition when the voids collapse at 0.8 GPa, whereas no phase transitions occur in the dihydrate, because its pores are supported by increased water content.

1. Introduction

Zinc plays a key role in the human body as a cofactor of numerous enzymes and it is therefore often included in dietary supplements and medicines for various illnesses (Shankar & Prasad, 1998; Haase et al., 2008; Roohani et al., 2013; Azeem et al., 2019). Zinc aspartate hydrate (ZnAsp₂·nH₂O, Asp denotes the aspartate anion; Fig. 1) is often used as a source of zinc cations and aspartate amino acids. This racemic complex preferentially crystallizes in the form of hydrates but their structures have not been determined so far.

Figure 1 The structural formula of zinc aspartate hydrate, ZnAsp2·nH2O.

We have established that crystallization from an aqueous solution under normal conditions yields the dihydrate, ZnAsp₂·2H₂O, whereas high-pressure crystallization yields the sesquihydrate, ZnAsp₂·1.5H₂O. The structures of both these hydrates are determined here, and the mechanism favouring reduced water content at high pressure is described.

The effect of high pressure on the hydration of various organic compounds, such as methane (Kevenvolden, 1995), thio­urea (Figuiere et al., 1975; Tomkowiak et al., 2013; Tomkowiak & Katrusiak, 2018), 1,4-di­aza­bicyclo[2.2.2]octane hydro­iodide (dabcoHI, Olejniczak & Katrusiak, 2010), 1,4-di­aza­bicyclo[2.2.2]octane dibromide (dabco2HBr, Andrzejewski et al., 2011), 5,6-di­methyl­benzimidazole (Zieliński & Katrusiak, 2015) and 4,4′-bipyrid­inium perchlorate (Anioła & Katrusiak, 2017), and minerals (Van Valkenburg et al., 1971), is well documented in the literature. However, in most cases high pressure increases the water content in a crystal structure, and exceptions are rare. For example, the hydrate Y₂(C₂O₄)₃·10H₂O reduces its water content at 1 GPa to Y₂(C₂O₄)₃·6H₂O (Zakharov et al., 2017), the dehydration of phosphatidylinositol bilayers was postulated above 0.7 GPa based on IR spectroscopy (Carrier & Wong, 1996), and the decomposition of orthoboric acid with the release of water at about 2 GPa was reported by Kuznetsov et al. (2006). We also noted that pressures above 1 GPa prevent the formation of hydrates of thio­urea (Figuiere et al., 1975; Tomkowiak et al., 2013; Tomkowiak & Katrusiak, 2018) and at pressures above 8 GPa no methane hydrates are formed (Kevenvolden, 1995). Presently, we have established that the porous crystals of ZnAsp₂·nH₂O display structural features connected to their water content. These features can be conveniently studied and modelled for this compound. We show that sesquihydrate ZnAsp₂·nH₂O can be employed as an internal component (in tablets) to protect active pharmaceutical ingredients (APIs) from the effects of humidity.

High-pressure studies on APIs increased the number of efficient methods for obtaining new polymorphs (Zakharov et al., 2016a,b; Neumann et al., 2015; Boldyreva et al., 2002; Boldyreva, 2003; Patyk-Kaźmierczak & Kaźmierczak, 2020; Fabbiani & Pulham, 2006; Oswald et al., 2010) and solvates (Fabbiani et al., 2003; 2014). Solvated APIs can be sensitive to the pressure employed in the process of formulation, for example in pressing tablets. High-pressure studies also provide a broader perspective for understanding the thermodynamic transformations of APIs.

2. Experimental

We performed high-pressure experiments either by gradually compressing a single crystal in a diamond anvil cell (DAC), or by high-pressure recrystallization and growing single crystals in isothermal and isochoric conditions from aqueous solutions in situ in the DAC. Experimental parameters and crystal data are listed in Table 1, and in Tables S1 and S2 in the supporting information. High-pressure experiments were performed in a Merrill–Bassett DAC (Merrill & Bassett, 1974), modified by mounting the anvils directly on steel backing plates with conical windows (Katrusiak, 2008). The form of the crystals grown was determined by single-crystal X-ray diffraction (Table 1, and Tables S1 and S2 in the supporting information). All isochoric high-pressure recrystallizations yielded the sesquihydrate, ZnAsp₂·1.5H₂O. Its growth process is illustrated in Fig. 2 (see also Fig. S1 in the supporting information).

Figure 2 The stages of ZnAsp2·1.5H2O single-crystal growth from aqueous solution under isochoric conditions in the DAC chamber. (a) Spontaneous powder precipitation at 433 K, and one seed at (b) 443 K, (c) 343 K and (d) 0.49 GPa/296 K. The ruby chip for pressure calibration lies near the middle of the chamber.

The sesquihydrate could be recovered from the DAC and no visible changes occurred to the samples exposed to air for weeks. On the other hand, the initially crystallized dihydrate powder kept in a thermally closed plastic bag for two months fully transformed into the sesquihydrate. This indicates that the dihydrate is stable only when submerged in water and in highly humid environments.

The compression of ZnAsp₂·1.5H₂O and ZnAsp₂·2H₂O crystals was determined for the samples mounted in the DAC. The gasket was made of 0.2 mm thick Inconel foil and the initial diameter of the spark-eroded hole was 0.45 mm. Glycerine was used as a hydro­static medium. The pressure in the DAC was calibrated before and after each diffraction measurement by the ruby fluorescence method (Piermarini et al., 1975; Mao et al., 1986) using a Photon Control Inc. spectrometer of enhanced resolution, affording an accuracy of 0.02 GPa.

Single-crystal high-pressure data were measured on a KUMA KM4 CCD diffractometer according to the procedure described previously (Budzianowski & Katrusiak, 2004). The CrysAlisPro software (Rigaku Oxford Diffraction, 2015) was used for diffraction data collection and preliminary reduction. Reflections that overlapped with diamond reflections were eliminated, and corrections for the DAC and sample absorption and for beam shadowing by the gasket were applied. Using OLEX2 (Dolomanov et al., 2009), the crystal structures were solved by intrinsic phasing with SHELXT (Sheldrick, 2015a) and refined by least-squares with the program SHELXL (Sheldrick, 2015b). The ambient-pressure structures were used as the starting models for refinement of the high-pressure data. Anisotropic displacement factors were generally applied for non-hydrogen atoms. C- and N-bound H atoms were located from the molecular geometry (assuming distances of C—H = 0.97 Å for methyl­ene, C—H = 0.98 Å for methine and N—H = 0.89 Å for NH₃). The water H atoms were located from difference Fourier maps and then the positions of H₂O were refined as rigid units. The U_iso values of the H atoms were constrained to 1.2 times the U_eq of their carrier atoms. Structural drawings were prepared using the program Mercury CSD 3.3 (Macrae et al., 2020). A total of 26 different data sets were collected, at 15 different pressures for the sesquihydrate and 11 different pressures for the dihydrate. The crystal data have been deposited in the Cambridge Structural Database (CSD; Groom et al., 2016) as supplementary publications (CSD 1972145–1972170).

Powder X-ray diffraction (XRPD) patterns were recorded using a Bruker AXS D8 Advance diffractometer, equipped with a sealed X-ray tube, a Johansson monochromator selecting Cu Kα₁ radiation (λ = 1.54060 Å) and a LynxEye detector. The samples were gently pressed into a flat round cuvette of about 0.4 cm³ in volume. The cuvette was rotated during the measurements, performed in θ steps of 0.02° and in the θ–2θ mode.

Thermogravimetric (TG) and differential scanning calorimetry (DSC) analyses were performed for 18.2 mg of ZnAsp₂·2H₂O in an N₂ atmosphere on a Setsys 1200 Setaram instrument between 293 K and 573 K at a scan speed of 5 K min⁻¹.

3. Results and discussion

The compressed crystals of ZnAsp₂·1.5H₂O and ZnAsp₂·2H₂O retain the ambient-pressure monoclinic symmetry of space group C2/c and triclinic symmetry of space group , respectively, up to 4 GPa at least (Table 1, Fig. 3, Figs. S2 and S3).

Table 1
Selected crystal data for ZnAsp₂·1.5H₂O and ZnAsp₂·2H₂O, all at 296 K (see also Tables S1 and S2 in the supporting information)

	ZnAsp2·1.5H2O		ZnAsp2·2H2O
Pressure (GPa)	0.0001	3.92	0.0001	4.02
Crystal system	Monoclinic	Monoclinic	Triclinic	Triclinic
Space group	C2/c	C2/c
a (Å)	16.2789 (3)	15.550 (3)	8.7873 (3)	8.343 (7)
b (Å)	10.7307 (2)	10.2262 (7)	9.5061 (3)	8.947 (6)
c (Å)	14.5393 (3)	13.966 (1)	9.8114 (3)	9.537 (3)
α (°)	90	90	111.784 (3)	110.02 (4)
β (°)	93.017 (2)	92.62 (3)	105.625 (3)	104.76 (4)
γ (°)	90	90	107.721 (3)	109.16 (7)
V (Å^3)	2536.26 (8)	2219 (4)	653.73 (4)	575.2 (7)
Z/Z′	4/0.5	4/0.5	1/0.5	1/0.5
Dx (g cm^−3)	1.868	2.135	1.857	2.111

Figure 3 Unit-cell dimensions of (a) ZnAsp2·1.5H2O (open symbols, dashed lines) and (b) ZnAsp2·2H2O (solid symbols and lines), relative to their values at 296 K/0.1 MPa, as a function of pressure. The magnitudes of the unit-cell parameters, including the angular dimensions, are plotted in Figs. S2 and S3. The vertical dashed line in panel (a) indicates the phase transition in ZnAsp2·1.5H2O (see also Fig. S6). The open black symbols in panel (b) show the volume compression in ZnAsp2·1.5H2O relative to the volume of ZnAsp2·2H2O at 0.1 MPa.

Although seemingly very different (Table 1), the crystal structures of ZnAsp₂ dihydrate and sesquihydrate are strikingly similar. Their Bravais lattices can be transformed into one another through the following matrix M:

where the subscripts m and t refer to the (pseudo)monoclinic C lattice of (ZnAsp₂·1.5H₂O) and the triclinic P lattice of (ZnAsp₂·2H₂O), respectively. The reverse matrix M⁻¹ transforms the lattice C_m into P_t:

Thus the triclinic P unit cell of ZnAsp₂·2H₂O at 0.1 MPa can be represented as the pseudo-monoclinic unit cell C, having the following dimensions: a = 16.445 Å, b = 10.804 Å, c = 14.780 Å, α = 85.28°, β = 92.27°, γ = 89.66°, which are similar to the unit cell of ZnAsp₂·1.5H₂O (Table 1). According to the unit-cell angles of the pseudo-monoclinic C lattice of ZnAsp₂·2H₂O (Fig. S3), with increasing pressure this triclinic structure only hardly, within about 0.5°, changes its distortions from the monoclinic symmetry.

Thus the sorption of water molecules into the ZnAsp₂·nH₂O framework results in its transformation, changing the symmetry of the crystal structure. It is characteristic that the monoclinic symmetry of space group C2/c of ZnAsp₂·1.5H₂O is reduced to the triclinic space group of ZnAsp₂·2H₂O after the water content increases. This inverse sorption–symmetry relation is surprising, as according to our survey an increased water content of the pores either increases or preserves the crystal symmetry. For example, the space-group symmetry R3 of anhydrate stepanovite polymorph ST1d increases to space group R3c for stepanovite [Mg(H₂O)₆][NaFe(C₂O₄)₃]·3H₂O; for the polymorph ST2d its anhydrate has space-group symmetry P3 and after hydration the symmetry increases to P3c (Huskić et al., 2019); the space-group symmetries P2₁/n and of lithium acetate (LiC₂H₃O₂) polymorphs increase to Cmmm for the dihydrate; and space group of lithium acetate monohydrate, 4(LiC₂H₃O₂)·H₂O, increases to P2₁/c for the tetrahydrate 4(LiC₂H₃O₂)·4H₂O (Martínez-Casado et al., 2011).

We have established that ZnAsp₂ preferentially crystallizes as the dihydrate when crystallized from water solution under normal conditions (298 K, 0.1 MPa). The dihydrate crystals are triclinic (Table 1). In these crystal structures the water molecules are located in channel pores and do not participate in the Zn²⁺ coordination. In ZnAsp₂·2H₂O the Zn²⁺ cation is coordinated by four carboxyl­ate oxygens of four Asp anions, as illustrated in Fig. 4. Each Asp participates in coordinating two Zn²⁺ cations, closing cyclamers of the form –Zn²⁺–Asp–Zn²⁺–Asp–, and these are combined into chains extending along the [010] crystal direction. In ZnAsp₂·1.5H₂O the Zn²⁺ cation is coordinated in the same way as in ZnAsp₂·2H₂O. The ZnAsp₂ ribbons are very similar in the dihydrate and sesquihydrate, as shown in Fig. 4. The conformation of the Asp units and their coordination of Zn²⁺ is consistent to within a few degrees for the corresponding torsion angles (Fig. S4).

Figure 4 (a) Autostereographic projections (Katrusiak, 2001) of the ribbons formed by the Zn cations four-fold coordinated by Asp anions in ZnAsp2·1.5H2O and ZnAsp2·2H2O. Water molecules have been omitted for clarity. (b) The ZnAsp2·1.5H2O and ZnAsp2·2H2O structures projected down the ZnAsp2 ribbons. Water molecules are represented as red balls. H atoms have been omitted for clarity.

It is a common feature of both ZnAsp₂·1.5H₂O and ZnAsp₂·2H₂O that all water molecules interact through O—H⋯O and N—H⋯O hydrogen bonds, but no water mol­ecules participate in Zn coordination. There are very similar intramolecular N13—H13C⋯O11 and N3—H3A⋯O2 hydrogen bonds in both ZnAsp₂·1.5H₂O and ZnAsp₂·2H₂O. Almost all of the hydrogen bonds involve water molecules. The hydrogen bonds to H₂O molecules are O1W—H1WB⋯O14, O1W—H1WA⋯O2, O2W—H2WB⋯O12 and N3—H3C⋯O1W. Two other hydrogen bonds are N13—H13B⋯O2 and N3—H3B⋯O13, both present in the ZnAsp₂·1.5H₂O and ZnAsp₂·2H₂O structures. The O2W—H2WA⋯O1W bond between two water molecules is formed only in ZnAsp₂·2H₂O (Figs. S5 and S9).

It is remarkable that although ZnAsp₂·2H₂O and ZnAsp₂·1.5H₂O can interconvert one into the other under ambient conditions, each of them can be compressed in glycerine to 4 GPa at least (Fig. 3). However, while the compression of ZnAsp₂·2H₂O is monotonic, in ZnAsp₂·1.5H₂O we have noted an anomalous strain at about 0.8 GPa. This anomaly is clearly seen in the pressure dependence of the monoclinic angle β, which initially rises and at 0.8 GPa drops abruptly by 0.1°, and then it continues to drop in a monotonous way it at still higher pressure (Fig. 5). A similar discontinuity is observed in the compression of unit-cell parameter a [Fig. 5(b)] and in the volume compression (Fig. 3). It appears that the anomalous `compression' of the β angle in ZnAsp₂·1.5H₂O is a consequence of the directional interactions – Zn—O coordination and O—H⋯O hydrogen bonds – forming the framework in this structure. These directional bonds play a dominant role in the dimensions and elastic properties of the crystal. Owing to this relatively rigid framework, some small voids are present in the crystal under normal conditions. However, above 0.8 GPa the directional bonds yield under the external pressure and the small voids are suppressed. Thus the anomalous compression marks the pressure value at which central forces supported by the external pressure overcome the angular dimensions favoured by the directional interactions, triggering a collapse to a more densely packed structure [Fig. 6(a)]. These two phases of ZnAsp₂·1.5H₂O will be further referred to as phases α and β.

Figure 5 The pressure dependence of (a) angle β and (b) parameter a of the unit cell in ZnAsp2·1.5H2O. The changes in all the unit-cell dimensions are plotted in Fig. S2.

Figure 6 (a) The pressure dependence of the void volume (Vvoids) of ZnAsp2·1.5H2O (open symbols, dotted lines) and ZnAsp2·2H2O (solid symbols, continuous line) after removing the water molecules from these structures, per one formula unit (Vvoids/Z). The void volume was calculated using the program Mercury (Macrae et al., 2020) with a probing-sphere radius of 1.2 Å and 0.1 Å steps. (b) The molecular volume of water (i.e. one H2O molecule in liquid; Bridgman, 1935) and ices VI (Kuhs et al., 1984) and VII (Bezacier et al., 2014) as a function of pressure compared with the difference in molecular volume (Vm = V/Z) between ZnAsp2·2H2O and ZnAsp2·1.5H2O (ΔVm). Δ0 is this difference at 0.1 MPa (see also Fig. S6).

The ZnAsp₂·1.5H₂O structure determined at 0.9 GPa is an average of these phases, as the X-ray diffraction measurement was performed when the sample had partly transformed between phases α and β. The anomalous compression at 0.8 GPa, determined from the unit-cell dimensions, agrees well with the collapse of the pores. Their volume is plotted as a function of pressure in Fig. 6 (note the `intermediate' volume of the pores at 0.9 GPa, due to the averaged structures of phases α and β, as explained above). According to the X-ray diffraction data, the transition at 0.8 GPa does not change the crystal symmetry. Thus it can be classified as an isostructural phase transition, which is quite common for metal–organic frameworks under pressure. For example, at 0.40 GPa Cd(APP)₂NO₃·NO₃ transforms between monoclinic phases, both of space-group symmetry P2₁/c (Półrolniczak et al., 2018) and Co₂(4,4′-bpy)₃(NO₃)₄·xH₂O preserves its orthorhombic space group Ccca at p_c = 6 GPa (Zhou et al., 2014), plus other known examples (Moggach et al., 2009; McKellar & Moggach, 2015; Sobczak et al., 2018; Bhattacharyya et al., 2019).

Interestingly, the subtraction of the molecular volume of ZnAsp₂·1.5H₂O from that of ZnAsp₂·2H₂O (denoted ΔV_m) should give the volume difference corresponding to half of the molecular volume of water [Fig. 6(b)]. The comparison of ΔV_m with the volume of one H₂O molecule in water and ices shows that there is more space in the pores than required for the accommodated water molecules, which explains the reason for the collapse of the pores. The work contribution to the Gibbs free energy at the transition in ZnAsp₂·1.5H₂O is 3.1 kJ mol⁻¹, compared with the work energy of 4.9 kJ mol⁻¹ performed by the pressure to compress phase α from 0.1 MPa to 0.8 GPa. The volume difference between ZnAsp₂·2H₂O and ZnAsp₂·1.5H₂O at 0.1 MPa is consistent with the broad distribution of the volume of solvent water occurring in organic pharmaceuticals (Glasser, 2019).

4. Practical implications

The subtle balance of water content in these two hydrates of zinc aspartate (ZnAsp₂) has implications for its use as a pharmaceutical agent. The undesired release of water in tablets results in their degradation, as illustrated in the photograph in Fig. 7. These undesired effects can be avoided by using zinc aspartate in the form of the sesquihydrate, ZnAsp₂·1.5H₂O, which is more stable and does not release or absorb water. The sesquihydrate can be obtained either by drying the dihydrate precipitate obtained from aqueous solution, or by performing the crystallization under high-pressure conditions. The high pressure of about 50 MPa required for this purpose is technologically attainable for larger amounts of the sample, although it would require some safety measures. High-pressure crystallization could be more advantageous in terms of the time needed to obtain the required product. Thus the high-pressure crystallization of zinc aspartate can be regarded as a potential candidate for pharmaceutical applications of high pressure (see also Fabbiani et al., 2014).

Figure 7 Tablets containing ZnAsp2·2H2O, some of which show clear signs of the release of water on the spontaneous transformation to ZnAsp2·1.5H2O: in the eight tablets grouped on the right-hand side of the photograph the degradation is visible as a beige shade and swelling, which leads to their easy abrasion and crushing.

5. Conclusions

We have established that the sesquihydrate ZnAsp₂·1.5H₂O is a stable form of the zinc aspartate complex (ZnAsp₂) under ambient conditions. We have shown that the precipitate obtained by crystallization from aqueous solution is the dihydrate, ZnAsp₂·2H₂O. The crystal structures of the sesquihydrate ZnAsp₂·1.5H₂O and the dihydrate ZnAsp₂·2H₂O are closely related, despite their different space-group symmetries.

The most eminent feature of these structures is that they form frameworks containing channel pores that are occupied by water molecules. The water molecules can enter the pores of the sesquihydrate ZnAsp₂·1.5H₂O when it is immersed in water, or leave the pores when the dihydrate ZnAsp₂·2H₂O is exposed to the air. This transformation of the dihydrate into the sesquihydrate is a slow process, taking days or weeks depending on the volume of the sample, its container, the size of the crystal grains, the humidity of the air, ventilation, temperature and other relevant parameters. Thus it is recommended to check whether the transformation into the sesquihydrate has been completed before further processing, for example granulating or tabletting.

The sesquihydrate can also be obtained directly by high-pressure crystallization. We found that an applied pressure as low as 50 MPa favours crystallization of the sesquihydrate from aqueous solution at 298 K.

The subtle isostructural phase transition in ZnAsp₂·1.5H₂O illustrates the role of directional interactions in stabilizing porous structures. It can be postulated that the sesquihydrate is favoured by high pressure because it increases the close packing of molecules in the structure and destabilizes the directional interactions, like hydrogen bonds, which bind the water molecules into the pores. However, it is apparent from other reverse effects on other hydrates that the pressure effects are quite complex and depend on specific structural features.

It should be noted that all our attempts to recrystallize racemic ZnAsp₂ hydrates never resulted in the separation of enantiomers. This negative result is consistent with the effect of pressure on other racemic mixtures of enantiomers reported so far (e.g. Jacques et al., 1994; Rietveld et al., 2011; Cai et al., 2013; Marciniak et al., 2014; Ostrowska et al., 2015; Wang et al., 2015; Ernst, 2018; Hochberg & Cintas, 2018; Roszak & Katrusiak, 2018).

Supporting information

Computing details

Program(s) used to solve structure: ShelXT (Sheldrick, 2015) for Zn-aspartate_sesquihydrate_0_001GPa, Zn-aspartate_sesquihydrate_0_29GPa, Zn-aspartate_sesquihydrate_0_49GPa, Zn-aspartate_sesquihydrate_0_79GPa, Zn-aspartate_sesquihydrate_1_44GPa, Zn-aspartate_sesquihydrate_1_82GPa, Zn-aspartate_sesquihydrate_2_49GPa, Zn-aspartate_dihydrate_0_001GPa, Zn-aspartate_dihydrate_0_05GPa, Zn-aspartate_dihydrate_0_15GPa, Zn-aspartate_dihydrate_0_40GPa, Zn-aspartate_dihydrate_0_70GPa, Zn-aspartate_dihydrate_1_02GPa, Zn-aspartate_dihydrate_1_54GPa, Zn-aspartate_dihydrate_2_53GPa, Zn-aspartate_dihydrate_3_05GPa, Zn-aspartate_dihydrate_3_53GPa; SHELXS (Sheldrick, 2008) for Zn-aspartate_sesquihydrate_0_05GPa, Zn-aspartate_sesquihydrate_0_85GPa, Zn-aspartate_sesquihydrate_1_15GPa, Zn-aspartate_sesquihydrate_1_62GPa, Zn-aspartate_sesquihydrate_2_15GPa, Zn-aspartate_sesquihydrate_2_91GPa, Zn-aspartate_sesquihydrate_3_54GPa, Zn-aspartate_sesquihydrate_3_92GPa, Zn-aspartate_dihydrate_4_02GPa. For all structures, program(s) used to refine structure: SHELXL (Sheldrick, 2015); molecular graphics: Olex2 (Dolomanov et al., 2009); software used to prepare material for publication: Olex2 (Dolomanov et al., 2009).

(Zn-aspartate_sesquihydrate_0_001GPa)

Crystal data

C16H24N4O16Zn2·3(H2O)	F(000) = 1464
Mr = 713.18	Dx = 1.868 Mg m^−3
Monoclinic, C2/c	Cu Kα radiation, λ = 1.54184 Å
a = 16.2789 (3) Å	Cell parameters from 2468 reflections
b = 10.7307 (2) Å	θ = 5.4–76.2°
c = 14.5393 (3) Å	µ = 3.23 mm^−1
β = 93.017 (2)°	T = 296 K
V = 2536.26 (8) Å^3	Plate, colourless
Z = 4	0.15 × 0.10 × 0.02 mm

Data collection

Multiwire proportional diffractometer	2468 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.020
Graphite monochromator	θmax = 76.2°, θmin = 5.4°
ω scan	h = −15→20
Absorption correction: integration integration	k = −13→12
Tmin = 0.712, Tmax = 0.937	l = −18→17
10199 measured reflections	62 standard reflections every 24 reflections
2632 independent reflections	intensity decay: none

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.030	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.086	w = 1/[σ^2(Fo^2) + (0.0487P)^2 + 2.529P] where P = (Fo^2 + 2Fc^2)/3
S = 1.11	(Δ/σ)max < 0.001
2632 reflections	Δρmax = 0.60 e Å^−3
196 parameters	Δρmin = −0.40 e Å^−3
2 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00025 (5)

Special details

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.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.730510 (15)	0.50404 (2)	0.449948 (17)	0.02585 (12)
O4	0.67955 (8)	0.87379 (13)	0.55387 (10)	0.0342 (3)
O2	0.54889 (8)	0.76159 (13)	0.39793 (10)	0.0321 (3)
O1	0.63918 (9)	0.60880 (14)	0.40487 (10)	0.0334 (3)
O14	0.76009 (9)	0.04837 (15)	0.41962 (10)	0.0363 (3)
O11	0.75421 (9)	0.37497 (15)	0.36264 (12)	0.0414 (4)
O13	0.87616 (10)	0.14571 (16)	0.45899 (10)	0.0412 (4)
O12	0.62930 (9)	0.33025 (16)	0.30225 (12)	0.0432 (4)
O3	0.57758 (11)	1.00639 (13)	0.58153 (14)	0.0420 (4)
N13	0.89140 (10)	0.25231 (16)	0.29576 (11)	0.0311 (3)
H13A	0.9032	0.2616	0.2371	0.037*
H13B	0.9359	0.2261	0.3282	0.037*
H13C	0.8752	0.3250	0.3180	0.037*
O1W	0.60744 (13)	0.98762 (17)	0.33339 (14)	0.0499 (4)
H1WA	0.6562	0.9951	0.3567	0.075*
H1WB	0.5871	0.9277	0.3629	0.075*
N3	0.46595 (11)	0.82054 (17)	0.56868 (13)	0.0365 (4)
H3A	0.4608	0.8449	0.5102	0.044*
H3B	0.4505	0.8821	0.6050	0.044*
H3C	0.4344	0.7541	0.5766	0.044*
O2W	0.5000	0.5206 (3)	0.2500	0.0659 (9)
H2W	0.537 (2)	0.466 (3)	0.255 (3)	0.075 (11)*
C1	0.59020 (10)	0.68141 (16)	0.44282 (13)	0.0248 (4)
C4	0.60666 (11)	0.90115 (17)	0.57328 (12)	0.0268 (4)
C11	0.70387 (11)	0.31174 (17)	0.31161 (13)	0.0269 (4)
C14	0.82094 (11)	0.11819 (17)	0.40240 (13)	0.0271 (4)
C12	0.74310 (11)	0.20731 (18)	0.25943 (13)	0.0278 (4)
H12A	0.7522	0.2363	0.1976	0.033*
H12B	0.7046	0.1383	0.2541	0.033*
C13	0.82431 (11)	0.15916 (17)	0.30241 (13)	0.0261 (4)
H13	0.8397	0.0860	0.2668	0.031*
C3	0.55298 (12)	0.78806 (18)	0.59243 (14)	0.0297 (4)
H3	0.5578	0.7727	0.6589	0.036*
C2	0.57929 (13)	0.66917 (17)	0.54510 (14)	0.0302 (4)
H2A	0.6308	0.6411	0.5746	0.036*
H2B	0.5385	0.6052	0.5546	0.036*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.02411 (17)	0.02488 (17)	0.02838 (18)	0.00207 (8)	−0.00019 (11)	−0.00047 (8)
O4	0.0268 (7)	0.0330 (7)	0.0429 (8)	−0.0037 (5)	0.0048 (6)	−0.0018 (6)
O2	0.0290 (7)	0.0285 (7)	0.0380 (7)	0.0052 (5)	−0.0052 (5)	0.0012 (6)
O1	0.0320 (7)	0.0375 (7)	0.0305 (7)	0.0123 (6)	0.0013 (5)	−0.0009 (6)
O14	0.0317 (7)	0.0413 (8)	0.0357 (7)	−0.0074 (6)	−0.0002 (6)	0.0096 (6)
O11	0.0280 (7)	0.0428 (8)	0.0530 (9)	0.0014 (6)	−0.0015 (6)	−0.0227 (7)
O13	0.0426 (8)	0.0467 (9)	0.0334 (7)	−0.0116 (7)	−0.0084 (6)	0.0068 (6)
O12	0.0260 (7)	0.0471 (9)	0.0557 (10)	0.0070 (6)	−0.0042 (6)	−0.0084 (7)
O3	0.0344 (8)	0.0262 (8)	0.0649 (11)	0.0005 (5)	−0.0023 (8)	−0.0007 (6)
N13	0.0239 (7)	0.0366 (9)	0.0328 (8)	0.0002 (6)	0.0021 (6)	0.0082 (7)
O1W	0.0480 (11)	0.0479 (10)	0.0543 (11)	−0.0098 (7)	0.0060 (8)	−0.0051 (8)
N3	0.0288 (8)	0.0345 (9)	0.0466 (10)	−0.0020 (7)	0.0048 (7)	−0.0059 (8)
O2W	0.0407 (15)	0.0475 (15)	0.107 (3)	0.000	−0.0200 (16)	0.000
C1	0.0195 (8)	0.0220 (8)	0.0327 (9)	−0.0016 (6)	−0.0015 (7)	−0.0010 (7)
C4	0.0269 (8)	0.0272 (9)	0.0257 (8)	−0.0017 (7)	−0.0024 (7)	−0.0003 (7)
C11	0.0257 (8)	0.0269 (9)	0.0281 (8)	0.0018 (7)	0.0007 (7)	0.0011 (7)
C14	0.0273 (9)	0.0235 (8)	0.0304 (9)	0.0027 (7)	0.0005 (7)	0.0017 (7)
C12	0.0267 (9)	0.0299 (9)	0.0265 (8)	0.0018 (7)	−0.0017 (7)	−0.0021 (7)
C13	0.0251 (8)	0.0256 (8)	0.0277 (9)	0.0025 (7)	0.0018 (7)	−0.0008 (7)
C3	0.0286 (9)	0.0267 (9)	0.0341 (9)	−0.0006 (7)	0.0056 (7)	−0.0022 (7)
C2	0.0339 (10)	0.0229 (8)	0.0343 (10)	0.0004 (7)	0.0060 (7)	0.0013 (7)

Geometric parameters (Å, º)

Zn1—O11	1.9313 (15)	O13—C14	1.223 (2)
Zn1—O1	1.9496 (14)	O12—C11	1.231 (2)
Zn1—O4^i	1.9682 (14)	O3—C4	1.233 (2)
Zn1—O14^ii	1.9762 (15)	N13—C13	1.487 (2)
O4—C4	1.269 (2)	N3—C3	1.482 (3)
O4—Zn1^i	1.9682 (14)	C1—C2	1.513 (3)
O2—C1	1.254 (2)	C4—C3	1.530 (3)
O1—C1	1.262 (2)	C11—C12	1.513 (3)
O14—C14	1.277 (2)	C14—C13	1.523 (3)
O14—Zn1^ii	1.9762 (15)	C12—C13	1.522 (2)
O11—C11	1.272 (2)	C3—C2	1.522 (3)
O11—Zn1—O1	111.58 (6)	O4—C4—C3	114.01 (16)
O11—Zn1—O4^i	106.53 (6)	O12—C11—O11	125.44 (18)
O1—Zn1—O4^i	99.31 (6)	O12—C11—C12	120.26 (17)
O11—Zn1—O14^ii	114.74 (7)	O11—C11—C12	114.29 (16)
O1—Zn1—O14^ii	120.39 (6)	O13—C14—O14	124.07 (18)
O4^i—Zn1—O14^ii	101.33 (6)	O13—C14—C13	120.72 (17)
C4—O4—Zn1^i	123.92 (13)	O14—C14—C13	115.08 (16)
C1—O1—Zn1	134.19 (13)	C11—C12—C13	115.20 (15)
C14—O14—Zn1^ii	109.47 (12)	N13—C13—C12	111.71 (15)
C11—O11—Zn1	128.38 (13)	N13—C13—C14	108.63 (15)
O2—C1—O1	121.99 (18)	C12—C13—C14	114.57 (15)
O2—C1—C2	118.94 (16)	N3—C3—C2	112.35 (16)
O1—C1—C2	119.05 (16)	N3—C3—C4	108.62 (16)
O3—C4—O4	127.02 (18)	C2—C3—C4	113.94 (16)
O3—C4—C3	118.89 (17)	C1—C2—C3	114.97 (16)
C1—C2—C3—N3	72.7 (2)	N13—C13—C14—O13	−11.5 (2)
C1—C2—C3—C4	−51.4 (2)	O12—C11—C12—C13	−156.33 (19)
N3—C3—C4—O3	30.6 (2)	Zn1—O1—C1—C2	−19.2 (3)
O2—C1—C2—C3	−28.1 (2)	Zn1—O11—C11—C12	−173.08 (14)
C11—C12—C13—N13	−69.7 (2)	Zn1—O4^i—C4^i—C3^i	167.31 (12)
C11—C12—C13—C14	54.4 (2)	Zn1—O14^ii—C14^ii—C13^ii	−176.44 (12)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1.

(Zn-aspartate_sesquihydrate_0_05GPa)

Crystal data

C16H24N4O16Zn2·3(H2O)	F(000) = 1464
Mr = 713.18	Dx = 1.889 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 16.210 (4) Å	Cell parameters from 351 reflections
b = 10.6863 (6) Å	θ = 3.8–26.4°
c = 14.4936 (9) Å	µ = 2.01 mm^−1
β = 92.95 (3)°	T = 296 K
V = 2507.3 (7) Å^3	Plate, colourless
Z = 4	0.20 × 0.20 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.024
Radiation source: sealed x-ray tube	θmax = 26.4°, θmin = 3.8°
ω scan	h = −3→2
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −12→13
Tmin = 0.675, Tmax = 0.904	l = −18→17
4042 measured reflections	12 standard reflections every 84 reflections
378 independent reflections	intensity decay: none
351 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.021	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.054	w = 1/[σ^2(Fo^2) + (0.0404P)^2 + 5.4767P] where P = (Fo^2 + 2Fc^2)/3
S = 1.10	(Δ/σ)max < 0.001
378 reflections	Δρmax = 0.11 e Å^−3
199 parameters	Δρmin = −0.11 e Å^−3
127 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 0.05 (2) GPa (50000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7318 (4)	0.50459 (6)	0.45038 (5)	0.024 (2)
O4	0.681 (3)	0.8726 (9)	0.5540 (5)	0.034 (3)
O2	0.5485 (13)	0.7608 (3)	0.3983 (3)	0.030 (5)
O1	0.639 (2)	0.6086 (4)	0.4051 (3)	0.030 (3)
O14	0.7580 (15)	0.0475 (5)	0.4184 (3)	0.036 (3)
O11	0.7551 (15)	0.3755 (4)	0.3623 (3)	0.044 (3)
O13	0.877 (2)	0.1447 (5)	0.4588 (3)	0.035 (5)
O12	0.626 (2)	0.3323 (8)	0.3014 (6)	0.049 (6)
O3	0.577 (2)	1.0065 (4)	0.5825 (5)	0.039 (5)
N13	0.888 (2)	0.2514 (5)	0.2948 (4)	0.030 (5)
H13A	0.9032	0.2616	0.2371	0.037*
H13B	0.9359	0.2261	0.3282	0.037*
H13C	0.8752	0.3250	0.3180	0.037*
O1W	0.6051 (17)	0.9874 (9)	0.3316 (8)	0.052 (5)
H1WA	0.657 (4)	0.994 (13)	0.338 (10)	0.063*
H1WB	0.593 (10)	0.928 (6)	0.367 (5)	0.063*
N3	0.469 (4)	0.8203 (10)	0.5689 (6)	0.037 (6)
H3A	0.4608	0.8449	0.5102	0.044*
H3B	0.4505	0.8821	0.6050	0.044*
H3C	0.4344	0.7541	0.5766	0.044*
O2W	0.500000	0.5205 (9)	0.250000	0.072 (6)
H2W	0.538 (7)	0.472 (6)	0.278 (5)	0.06 (4)*
C1	0.590 (4)	0.6807 (6)	0.4423 (5)	0.024 (3)
C4	0.607 (4)	0.9019 (9)	0.5728 (7)	0.023 (4)
C11	0.706 (4)	0.3138 (13)	0.3099 (8)	0.023 (4)
C14	0.820 (3)	0.1175 (6)	0.4020 (5)	0.022 (3)
C12	0.743 (3)	0.2076 (6)	0.2584 (4)	0.024 (3)
H12A	0.703756	0.139443	0.254129	0.029*
H12B	0.752479	0.235219	0.196003	0.029*
C13	0.823 (2)	0.1588 (6)	0.3011 (4)	0.025 (3)
H13	0.839066	0.085722	0.265171	0.030*
C3	0.554 (3)	0.7880 (10)	0.5930 (8)	0.06 (6)
H3	0.558567	0.773291	0.659759	0.075*
C2	0.5767 (19)	0.6678 (5)	0.5459 (4)	0.024 (3)
H2A	0.533177	0.607083	0.553838	0.029*
H2B	0.626809	0.635126	0.576370	0.029*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.027 (7)	0.0229 (5)	0.0231 (6)	−0.0005 (14)	−0.0012 (19)	−0.0007 (3)
O4	0.034 (7)	0.031 (3)	0.038 (3)	−0.001 (6)	0.005 (5)	−0.003 (3)
O2	0.031 (14)	0.0264 (19)	0.0316 (19)	0.010 (7)	−0.007 (6)	0.0045 (17)
O1	0.030 (7)	0.035 (2)	0.0256 (19)	0.004 (5)	0.001 (5)	−0.0013 (18)
O14	0.036 (7)	0.039 (2)	0.033 (2)	−0.001 (5)	0.002 (5)	0.010 (2)
O11	0.044 (7)	0.042 (2)	0.046 (2)	−0.001 (5)	−0.002 (5)	−0.021 (2)
O13	0.033 (14)	0.043 (2)	0.029 (2)	−0.005 (8)	0.000 (8)	0.005 (2)
O12	0.049 (15)	0.045 (5)	0.054 (5)	−0.004 (9)	0.002 (9)	−0.011 (3)
O3	0.037 (14)	0.027 (3)	0.052 (3)	0.007 (8)	0.014 (9)	−0.0010 (19)
N13	0.031 (14)	0.032 (3)	0.028 (3)	−0.007 (9)	0.007 (8)	0.006 (2)
O1W	0.053 (14)	0.043 (3)	0.061 (3)	−0.005 (8)	0.010 (9)	−0.006 (2)
N3	0.038 (14)	0.033 (5)	0.039 (4)	0.002 (10)	0.000 (10)	−0.005 (3)
O2W	0.072 (14)	0.044 (4)	0.099 (6)	0.000	−0.001 (10)	0.000
C1	0.024 (7)	0.021 (3)	0.027 (3)	−0.002 (6)	0.000 (6)	−0.001 (3)
C4	0.023 (8)	0.022 (5)	0.024 (4)	−0.002 (6)	0.002 (6)	−0.002 (3)
C11	0.023 (8)	0.023 (4)	0.024 (4)	0.000 (6)	0.001 (6)	0.001 (3)
C14	0.022 (7)	0.021 (3)	0.024 (3)	0.000 (5)	0.003 (5)	−0.001 (3)
C12	0.024 (7)	0.024 (2)	0.024 (3)	0.001 (5)	0.003 (5)	0.000 (2)
C13	0.024 (7)	0.024 (3)	0.026 (3)	−0.001 (5)	0.002 (5)	0.002 (2)
C3	0.13 (19)	0.024 (5)	0.035 (5)	−0.015 (17)	0.010 (19)	−0.001 (3)
C2	0.024 (7)	0.020 (2)	0.029 (3)	0.003 (5)	0.003 (5)	0.002 (2)

Geometric parameters (Å, º)

Zn1—O4^i	1.94 (4)	O12—C11	1.32 (8)
Zn1—O1	1.96 (3)	O3—C4	1.23 (3)
Zn1—O14^ii	1.980 (4)	N13—C13	1.45 (3)
Zn1—O11	1.930 (7)	N3—C3	1.44 (10)
O4—C4	1.28 (8)	C1—C2	1.535 (17)
O2—C1	1.25 (3)	C4—C3	1.52 (5)
O1—C1	1.24 (5)	C11—C12	1.50 (3)
O14—C14	1.29 (4)	C14—C13	1.531 (10)
O11—C11	1.26 (4)	C12—C13	1.50 (5)
O13—C14	1.23 (3)	C3—C2	1.509 (19)
O4^i—Zn1—O1	99.1 (12)	O3—C4—C3	119 (5)
O4^i—Zn1—O14^ii	101.3 (7)	O11—C11—O12	125 (2)
O1—Zn1—O14^ii	120.4 (8)	O11—C11—C12	116 (4)
O11—Zn1—O4^i	107.1 (9)	O12—C11—C12	119 (3)
O11—Zn1—O1	110.9 (5)	O14—C14—C13	114 (2)
O11—Zn1—O14^ii	115.1 (3)	O13—C14—O14	125.2 (11)
C4—O4—Zn1^i	122.5 (13)	O13—C14—C13	121 (3)
C1—O1—Zn1	134.4 (13)	C13—C12—C11	114.7 (19)
C14—O14—Zn1^ii	108.2 (11)	N13—C13—C14	108.4 (16)
C11—O11—Zn1	129 (2)	N13—C13—C12	110.5 (13)
O2—C1—C2	117 (3)	C12—C13—C14	115 (2)
O1—C1—O2	122.9 (10)	N3—C3—C4	107 (2)
O1—C1—C2	120 (2)	N3—C3—C2	110 (2)
O4—C4—C3	112.6 (19)	C2—C3—C4	116 (3)
O3—C4—O4	129 (4)	C3—C2—C1	114.6 (9)
Zn1—O4^i—C4^i—C3^i	167.4 (8)	N13—C13—C14—O13	−13 (3)
Zn1—O1—C1—C2	−22 (6)	N3—C3—C4—O3	32 (2)
Zn1—O14^ii—C14^ii—C13^ii	−176.6 (14)	C1—C2—C3—N3	75 (4)
Zn1—O11—C11—C12	−172.1 (9)	C1—C2—C3—C4	−47 (4)
O2—C1—C2—C3	−32 (4)	C11—C12—C13—N13	−68 (2)
O12—C11—C12—C13	−154.5 (19)	C11—C12—C13—C14	55 (2)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1.

(Zn-aspartate_sesquihydrate_0_29GPa)

Crystal data

C16H24N4O16Zn2·3(H2O)	F(000) = 1464
Mr = 713.18	Dx = 1.889 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 16.206 (3) Å	Cell parameters from 712 reflections
b = 10.6965 (4) Å	θ = 4.6–27.1°
c = 14.4922 (5) Å	µ = 2.01 mm^−1
β = 93.185 (8)°	T = 296 K
V = 2508.2 (5) Å^3	Plate, colourless
Z = 4	0.15 × 0.15 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.026
Radiation source: sealed x-ray tube	θmax = 27.1°, θmin = 4.6°
ω scan	h = −10→10
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −12→12
Tmin = 0.747, Tmax = 0.904	l = −18→17
5096 measured reflections	12 standard reflections every 84 reflections
823 independent reflections	intensity decay: none
712 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.030	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.080	w = 1/[σ^2(Fo^2) + (0.0408P)^2 + 7.4628P] where P = (Fo^2 + 2Fc^2)/3
S = 1.11	(Δ/σ)max = 0.001
823 reflections	Δρmax = 0.32 e Å^−3
200 parameters	Δρmin = −0.22 e Å^−3
32 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 0.29 (2) GPa (290000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.73109 (7)	0.50456 (5)	0.45041 (4)	0.0254 (7)
O4	0.6792 (5)	0.8729 (3)	0.5534 (3)	0.040 (4)
O2	0.5483 (4)	0.7615 (3)	0.3981 (3)	0.029 (3)
O1	0.6395 (4)	0.6085 (3)	0.4050 (3)	0.036 (4)
O14	0.7582 (5)	0.0480 (4)	0.4182 (3)	0.038 (4)
O11	0.7552 (5)	0.3760 (4)	0.3625 (3)	0.044 (4)
O13	0.8751 (5)	0.1447 (4)	0.4585 (3)	0.038 (4)
O12	0.6301 (6)	0.3312 (4)	0.3012 (4)	0.0492 (16)
O3	0.5767 (5)	1.0067 (3)	0.5819 (3)	0.042 (4)
N13	0.8919 (6)	0.2518 (5)	0.2953 (3)	0.035 (5)
H13A	0.9032	0.2616	0.2371	0.037*
H13B	0.9359	0.2261	0.3282	0.037*
H13C	0.8752	0.3250	0.3180	0.037*
O1W	0.6063 (7)	0.9871 (4)	0.3309 (4)	0.067 (5)
H1WA	0.6520	1.0165	0.3527	0.090*
H1WB	0.5985	0.9222	0.3631	0.090*
N3	0.4665 (9)	0.8202 (6)	0.5686 (5)	0.046 (7)
H3A	0.4608	0.8449	0.5102	0.044*
H3B	0.4505	0.8821	0.6050	0.044*
H3C	0.4344	0.7541	0.5766	0.044*
O2W	0.5000	0.5199 (7)	0.2500	0.071 (3)
H2W	0.554 (5)	0.475 (7)	0.246 (7)	0.14 (4)
C1	0.5882 (6)	0.6810 (5)	0.4419 (4)	0.029 (5)
C4	0.6084 (8)	0.9009 (5)	0.5740 (4)	0.029 (6)
C11	0.7038 (8)	0.3126 (5)	0.3108 (5)	0.028 (2)
C14	0.8204 (7)	0.1176 (5)	0.4015 (4)	0.0275 (14)
C12	0.7447 (11)	0.2080 (7)	0.2587 (5)	0.033 (7)
H12A	0.7057	0.1394	0.2514	0.040*
H12B	0.7551	0.2383	0.1974	0.040*
C13	0.8230 (9)	0.1581 (7)	0.3008 (4)	0.026 (7)
H13	0.8378	0.0846	0.2649	0.031*
C3	0.5521 (11)	0.7874 (7)	0.5924 (5)	0.034 (8)
H3	0.5565	0.7719	0.6591	0.041*
C2	0.5782 (6)	0.6686 (4)	0.5459 (3)	0.027 (5)
H2A	0.5374	0.6043	0.5560	0.032*
H2B	0.6303	0.6409	0.5752	0.032*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.023 (2)	0.0277 (6)	0.0251 (5)	0.0025 (3)	−0.0002 (8)	−0.0003 (2)
O4	0.050 (14)	0.034 (3)	0.037 (3)	−0.006 (2)	0.013 (5)	−0.0033 (17)
O2	0.026 (11)	0.026 (3)	0.034 (2)	0.005 (2)	−0.011 (4)	0.0025 (16)
O1	0.044 (13)	0.038 (3)	0.027 (2)	0.016 (3)	0.006 (5)	−0.0009 (15)
O14	0.031 (14)	0.049 (3)	0.035 (3)	−0.011 (3)	−0.002 (5)	0.0082 (18)
O11	0.031 (14)	0.048 (3)	0.051 (3)	0.000 (3)	−0.001 (6)	−0.025 (2)
O13	0.031 (15)	0.053 (3)	0.030 (3)	−0.010 (3)	−0.009 (5)	0.0084 (19)
O12	0.048 (3)	0.0484 (19)	0.051 (2)	0.0030 (19)	0.002 (2)	−0.0053 (15)
O3	0.038 (14)	0.024 (3)	0.063 (3)	0.003 (2)	−0.004 (5)	−0.0002 (17)
N13	0.034 (17)	0.040 (4)	0.031 (3)	−0.003 (3)	0.008 (6)	0.006 (2)
O1W	0.093 (16)	0.043 (4)	0.071 (4)	−0.013 (3)	0.039 (6)	−0.009 (2)
N3	0.05 (2)	0.036 (4)	0.047 (4)	−0.007 (4)	0.005 (8)	−0.007 (2)
O2W	0.070 (3)	0.066 (3)	0.077 (3)	0.000	0.001 (2)	0.000
H2W	0.14 (4)	0.14 (4)	0.14 (4)	0.000 (2)	0.008 (3)	0.000 (2)
C1	0.031 (16)	0.021 (4)	0.034 (3)	−0.008 (3)	0.004 (6)	−0.002 (2)
C4	0.04 (2)	0.032 (5)	0.019 (3)	−0.008 (4)	0.002 (7)	−0.002 (2)
C11	0.028 (5)	0.030 (3)	0.027 (3)	0.003 (3)	0.001 (4)	0.002 (2)
C14	0.0274 (19)	0.0274 (16)	0.0277 (16)	0.0007 (11)	0.0016 (11)	0.0002 (10)
C12	0.05 (2)	0.031 (5)	0.024 (4)	0.002 (4)	0.007 (9)	−0.001 (2)
C13	0.02 (2)	0.032 (5)	0.025 (4)	0.003 (4)	0.000 (9)	−0.001 (2)
C3	0.04 (3)	0.032 (5)	0.033 (4)	0.004 (4)	0.006 (9)	−0.001 (3)
C2	0.029 (16)	0.024 (4)	0.027 (3)	0.001 (3)	0.001 (6)	0.0011 (19)

Geometric parameters (Å, º)

Zn1—O4^i	1.960 (7)	N3—H3A	0.8900
Zn1—O1	1.940 (6)	N3—H3B	0.8900
Zn1—O14^ii	1.984 (4)	N3—H3C	0.8900
Zn1—O11	1.930 (4)	N3—C3	1.45 (2)
O4—C4	1.239 (13)	O2W—H2W	1.01 (5)
O2—C1	1.232 (9)	C1—C2	1.530 (7)
O1—C1	1.276 (8)	C4—C3	1.551 (16)
O14—C14	1.288 (10)	C11—C12	1.522 (9)
O11—C11	1.282 (13)	C14—C13	1.525 (8)
O13—C14	1.212 (12)	C12—H12A	0.9700
O12—C11	1.212 (15)	C12—H12B	0.9700
O3—C4	1.251 (8)	C12—C13	1.48 (2)
N13—H13A	0.8900	C13—H13	0.9800
N13—H13B	0.8900	C3—H3	0.9800
N13—H13C	0.8900	C3—C2	1.510 (8)
N13—C13	1.507 (17)	C2—H2A	0.9700
O1W—H1WA	0.8499	C2—H2B	0.9700
O1W—H1WB	0.8501
O4^i—Zn1—O14^ii	101.0 (2)	O12—C11—O11	125.7 (7)
O1—Zn1—O4^i	99.3 (2)	O12—C11—C12	121.2 (12)
O1—Zn1—O14^ii	120.8 (2)	O14—C14—C13	114.0 (10)
O11—Zn1—O4^i	106.3 (3)	O13—C14—O14	124.1 (5)
O11—Zn1—O1	111.3 (3)	O13—C14—C13	121.8 (9)
O11—Zn1—O14^ii	115.0 (2)	C11—C12—H12A	108.1
C4—O4—Zn1^i	122.9 (4)	C11—C12—H12B	108.1
C1—O1—Zn1	135.2 (4)	H12A—C12—H12B	107.3
C14—O14—Zn1^ii	108.4 (6)	C13—C12—C11	116.6 (11)
C11—O11—Zn1	127.9 (7)	C13—C12—H12A	108.1
H13A—N13—H13B	111.0	C13—C12—H12B	108.1
H13A—N13—H13C	109.5	N13—C13—C14	107.4 (10)
H13B—N13—H13C	109.5	N13—C13—H13	107.5
C13—N13—H13A	109.5	C14—C13—H13	107.5
C13—N13—H13B	109.5	C12—C13—N13	111.1 (7)
C13—N13—H13C	109.5	C12—C13—C14	115.5 (10)
H1WA—O1W—H1WB	104.5	C12—C13—H13	107.5
H3A—N3—H3B	109.5	N3—C3—C4	109.5 (7)
H3A—N3—H3C	109.5	N3—C3—H3	106.9
H3B—N3—H3C	109.5	N3—C3—C2	112.6 (12)
C3—N3—H3A	109.5	C4—C3—H3	106.9
C3—N3—H3B	109.5	C2—C3—C4	113.6 (9)
C3—N3—H3C	109.5	C2—C3—H3	106.9
O2—C1—O1	122.9 (5)	C1—C2—H2A	108.6
O2—C1—C2	119.2 (6)	C1—C2—H2B	108.6
O1—C1—C2	117.9 (6)	C3—C2—C1	114.5 (5)
O4—C4—O3	129.2 (8)	C3—C2—H2A	108.6
O4—C4—C3	114.5 (7)	C3—C2—H2B	108.6
O3—C4—C3	116.3 (10)	H2A—C2—H2B	107.6
O11—C11—C12	113.1 (12)
Zn1—O1—C1—C2	−17.2 (11)	N3—C3—C4—O3	29.4 (9)
Zn1—O11—C11—C12	−172.9 (4)	C1—C2—C3—N3	71.9 (11)
O2—C1—C2—C3	−26.4 (13)	C1—C2—C3—C4	−53.3 (13)
O12—C11—C12—C13	−155.1 (11)	C11—C12—C13—N13	−70.4 (9)
N13—C13—C14—O13	−10.9 (11)	C11—C12—C13—C14	52.2 (16)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1.

(Zn-aspartate_sesquihydrate_0_49GPa)

Crystal data

C16H24N4O16Zn2·3(H2O)	F(000) = 1464
Mr = 713.18	Dx = 1.907 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 16.191 (4) Å	Cell parameters from 692 reflections
b = 10.6521 (5) Å	θ = 9.2–54.5°
c = 14.4247 (6) Å	µ = 2.03 mm^−1
β = 93.183 (9)°	T = 296 K
V = 2484.0 (6) Å^3	Plate, colourless
Z = 4	0.30 × 0.30 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.025
Radiation source: sealed x-ray tube	θmax = 27.3°, θmin = 4.6°
ω scan	h = −10→10
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −12→12
Tmin = 0.549, Tmax = 0.903	l = −18→17
5033 measured reflections	12 standard reflections every 84 reflections
816 independent reflections	intensity decay: none
692 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.027	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.074	w = 1/[σ^2(Fo^2) + (0.0407P)^2 + 4.3878P] where P = (Fo^2 + 2Fc^2)/3
S = 1.11	(Δ/σ)max < 0.001
816 reflections	Δρmax = 0.30 e Å^−3
196 parameters	Δρmin = −0.17 e Å^−3
14 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 0.49 (2) GPa (490000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.73180 (7)	0.50506 (5)	0.45075 (4)	0.0258 (7)
O4	0.6789 (5)	0.8724 (3)	0.5528 (3)	0.037 (4)
O2	0.5477 (4)	0.7609 (3)	0.3982 (2)	0.026 (3)
O1	0.6392 (4)	0.6085 (3)	0.4055 (2)	0.039 (4)
O14	0.7566 (5)	0.0476 (3)	0.4173 (3)	0.043 (4)
O11	0.7557 (5)	0.3763 (4)	0.3617 (3)	0.039 (4)
O13	0.8743 (5)	0.1439 (3)	0.4586 (3)	0.035 (4)
O12	0.6298 (6)	0.3330 (4)	0.3006 (4)	0.038 (5)
O3	0.5761 (5)	1.0068 (3)	0.5830 (3)	0.042 (4)
N13	0.8915 (6)	0.2513 (4)	0.2946 (3)	0.036 (5)
H13A	0.9079	0.2549	0.2368	0.043*
H13B	0.9336	0.2272	0.3327	0.043*
H13C	0.8741	0.3267	0.3116	0.043*
O1W	0.6054 (6)	0.9869 (4)	0.3291 (4)	0.069 (4)
H1WA	0.6467	1.0253	0.3535	0.0803*
H1WB	0.5979	0.9261	0.3652	0.0803*
N3	0.4652 (8)	0.8197 (6)	0.5691 (4)	0.046 (6)
H3A	0.4593	0.8351	0.5085	0.055*
H3B	0.4514	0.8878	0.6005	0.055*
H3C	0.4324	0.7562	0.5833	0.055*
O2W	0.5000	0.5203 (6)	0.2500	0.064 (6)
H2W	0.555 (5)	0.478 (7)	0.249 (7)	0.085 (5)*
C1	0.5885 (6)	0.6811 (4)	0.4427 (4)	0.028 (4)
C4	0.6081 (7)	0.9003 (5)	0.5741 (4)	0.030 (6)
C11	0.7031 (10)	0.3133 (6)	0.3102 (6)	0.028 (2)
C14	0.8192 (7)	0.1173 (4)	0.4005 (4)	0.0271 (19)
C12	0.7437 (10)	0.2087 (6)	0.2572 (5)	0.034 (7)
H12A	0.7044	0.1403	0.2491	0.040*
H12B	0.7545	0.2400	0.1959	0.040*
C13	0.8214 (9)	0.1575 (6)	0.2993 (4)	0.029 (7)
H13	0.8359	0.0836	0.2631	0.035*
C3	0.5506 (10)	0.7870 (7)	0.5938 (5)	0.026 (7)
H3	0.5550	0.7719	0.6609	0.032*
C2	0.5775 (5)	0.6670 (4)	0.5467 (3)	0.031 (5)
H2A	0.5366	0.6023	0.5558	0.038*
H2B	0.6294	0.6390	0.5766	0.038*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.026 (2)	0.0263 (5)	0.0255 (4)	0.0022 (3)	0.0005 (8)	−0.0005 (2)
O4	0.041 (13)	0.034 (3)	0.038 (3)	−0.005 (2)	0.011 (4)	−0.0036 (16)
O2	0.016 (11)	0.029 (3)	0.033 (2)	0.006 (2)	−0.010 (4)	0.0031 (15)
O1	0.050 (12)	0.036 (3)	0.030 (2)	0.016 (2)	0.009 (5)	−0.0009 (15)
O14	0.045 (14)	0.047 (3)	0.036 (3)	−0.010 (3)	0.000 (5)	0.0087 (18)
O11	0.018 (14)	0.045 (3)	0.053 (3)	0.002 (3)	−0.005 (5)	−0.0244 (19)
O13	0.021 (14)	0.054 (3)	0.029 (3)	−0.007 (3)	−0.015 (5)	0.0095 (18)
O12	0.016 (17)	0.049 (3)	0.049 (3)	0.008 (3)	−0.010 (6)	−0.0070 (19)
O3	0.042 (14)	0.023 (3)	0.062 (3)	0.0031 (19)	0.000 (5)	−0.0003 (15)
N13	0.045 (16)	0.034 (3)	0.030 (3)	−0.001 (3)	0.014 (5)	0.005 (2)
O1W	0.102 (15)	0.037 (3)	0.073 (3)	−0.014 (2)	0.043 (6)	−0.0114 (19)
N3	0.06 (2)	0.032 (4)	0.042 (3)	−0.004 (4)	0.002 (7)	−0.007 (2)
O2W	0.05 (2)	0.043 (5)	0.102 (6)	0.000	−0.012 (9)	0.000
C1	0.029 (15)	0.020 (4)	0.034 (3)	−0.010 (3)	0.005 (6)	−0.003 (2)
C4	0.04 (2)	0.033 (4)	0.018 (3)	−0.010 (4)	−0.004 (6)	0.001 (2)
C11	0.026 (5)	0.029 (3)	0.028 (3)	0.006 (3)	0.001 (4)	0.003 (2)
C14	0.027 (5)	0.025 (2)	0.030 (3)	0.002 (2)	0.002 (3)	0.002 (2)
C12	0.04 (2)	0.031 (5)	0.027 (4)	0.004 (4)	0.013 (8)	0.000 (2)
C13	0.04 (2)	0.022 (4)	0.028 (4)	0.000 (3)	0.008 (8)	0.000 (2)
C3	0.01 (3)	0.034 (5)	0.034 (4)	0.005 (4)	0.004 (8)	−0.002 (2)
C2	0.044 (16)	0.021 (3)	0.030 (3)	0.000 (3)	0.007 (6)	0.0010 (18)

Geometric parameters (Å, º)

Zn1—O4^i	1.950 (6)	N3—H3A	0.8900
Zn1—O1	1.944 (6)	N3—H3B	0.8900
Zn1—O14^ii	1.983 (4)	N3—H3C	0.8900
Zn1—O11	1.933 (4)	N3—C3	1.45 (2)
O4—C4	1.240 (12)	O2W—H2W	1.00 (5)
O2—C1	1.234 (9)	C1—C2	1.528 (6)
O1—C1	1.268 (8)	C4—C3	1.559 (15)
O14—C14	1.291 (10)	C11—C12	1.522 (8)
O11—C11	1.287 (17)	C14—C13	1.523 (7)
O13—C14	1.223 (11)	C12—H12A	0.9700
O12—C11	1.206 (19)	C12—H12B	0.9700
O3—C4	1.257 (8)	C12—C13	1.47 (2)
N13—H13A	0.8900	C13—H13	0.9800
N13—H13B	0.8900	C3—H3	0.9800
N13—H13C	0.8900	C3—C2	1.523 (7)
N13—C13	1.516 (16)	C2—H2A	0.9700
O1W—H1WA	0.8444	C2—H2B	0.9700
O1W—H1WB	0.8441
O4^i—Zn1—O14^ii	100.6 (2)	O12—C11—O11	126.2 (7)
O1—Zn1—O4^i	99.8 (2)	O12—C11—C12	121.3 (14)
O1—Zn1—O14^ii	120.8 (2)	O14—C14—C13	113.7 (9)
O11—Zn1—O4^i	106.3 (2)	O13—C14—O14	123.6 (5)
O11—Zn1—O1	111.0 (3)	O13—C14—C13	122.6 (8)
O11—Zn1—O14^ii	115.2 (2)	C11—C12—H12A	108.1
C4—O4—Zn1^i	122.9 (4)	C11—C12—H12B	108.1
C1—O1—Zn1	135.2 (4)	H12A—C12—H12B	107.3
C14—O14—Zn1^ii	108.0 (5)	C13—C12—C11	116.6 (11)
C11—O11—Zn1	127.1 (8)	C13—C12—H12A	108.1
H13A—N13—H13B	109.5	C13—C12—H12B	108.1
H13A—N13—H13C	109.5	N13—C13—C14	106.5 (9)
H13B—N13—H13C	109.5	N13—C13—H13	107.6
C13—N13—H13A	109.5	C14—C13—H13	107.6
C13—N13—H13B	109.5	C12—C13—N13	111.3 (6)
C13—N13—H13C	109.5	C12—C13—C14	115.8 (9)
H1WA—O1W—H1WB	104.7	C12—C13—H13	107.6
H3A—N3—H3B	109.5	N3—C3—C4	109.9 (7)
H3A—N3—H3C	109.5	N3—C3—H3	107.2
H3B—N3—H3C	109.5	N3—C3—C2	112.6 (11)
C3—N3—H3A	109.5	C4—C3—H3	107.2
C3—N3—H3B	109.5	C2—C3—C4	112.4 (8)
C3—N3—H3C	109.5	C2—C3—H3	107.2
O2—C1—O1	122.7 (4)	C1—C2—H2A	108.7
O2—C1—C2	119.4 (5)	C1—C2—H2B	108.7
O1—C1—C2	117.9 (6)	C3—C2—C1	114.0 (4)
O4—C4—O3	129.3 (7)	C3—C2—H2A	108.7
O4—C4—C3	115.4 (6)	C3—C2—H2B	108.7
O3—C4—C3	115.3 (9)	H2A—C2—H2B	107.6
O11—C11—C12	112.4 (14)
Zn1—O1—C1—C2	−19.4 (10)	N3—C3—C4—O3	31.0 (8)
Zn1—O11—C11—C12	−172.9 (4)	C1—C2—C3—N3	72.1 (10)
O2—C1—C2—C3	−27.9 (12)	C1—C2—C3—C4	−52.6 (12)
O12—C11—C12—C13	−155.2 (11)	C11—C12—C13—N13	−70.6 (9)
N13—C13—C14—O13	−10.8 (10)	C11—C12—C13—C14	51.2 (16)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1.

(Zn-aspartate_sesquihydrate_0_79GPa)

Crystal data

C16H24N4O16Zn2·3(H2O)	F(000) = 1464
Mr = 713.18	Dx = 1.929 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 16.098 (2) Å	Cell parameters from 571 reflections
b = 10.605 (2) Å	θ = 3.7–26.9°
c = 14.405 (2) Å	µ = 2.06 mm^−1
β = 93.218 (16)°	T = 296 K
V = 2455.3 (7) Å^3	Plate, colourless
Z = 4	0.20 × 0.15 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.064
Radiation source: sealed x-ray tube	θmax = 26.9°, θmin = 3.7°
ω scan	h = −18→18
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −10→10
Tmin = 0.698, Tmax = 0.902	l = −15→15
4921 measured reflections	12 standard reflections every 84 reflections
824 independent reflections	intensity decay: none
571 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.062	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.199	w = 1/[σ^2(Fo^2) + (0.1168P)^2 + 15.7225P] where P = (Fo^2 + 2Fc^2)/3
S = 1.15	(Δ/σ)max < 0.001
824 reflections	Δρmax = 0.44 e Å^−3
196 parameters	Δρmin = −0.44 e Å^−3
32 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 0.79 (2) GPa (790000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.73234 (10)	0.50539 (16)	0.45125 (12)	0.0332 (8)
O4	0.6772 (5)	0.8718 (10)	0.5519 (7)	0.041 (3)
O2	0.5478 (6)	0.7613 (11)	0.3980 (7)	0.032 (3)
O1	0.6400 (6)	0.6080 (10)	0.4060 (7)	0.042 (3)
O14	0.7553 (7)	0.0453 (11)	0.4166 (7)	0.053 (3)
O11	0.7553 (6)	0.3770 (13)	0.3601 (9)	0.051 (4)
O13	0.8728 (8)	0.1429 (13)	0.4587 (9)	0.053 (4)
O12	0.6285 (7)	0.3329 (9)	0.2995 (8)	0.049 (3)
O3	0.5758 (6)	1.0055 (10)	0.5822 (8)	0.045 (3)
N13	0.8913 (7)	0.2536 (12)	0.2936 (8)	0.037 (3)
H13A	0.9036	0.2635	0.2346	0.044*
H13B	0.9364	0.2276	0.3269	0.044*
H13C	0.8742	0.3267	0.3161	0.044*
O1W	0.6014 (9)	0.9870 (15)	0.3282 (9)	0.076 (5)
H1WA	0.6435	1.0264	0.3494	0.114*
H1WB	0.5890	0.9389	0.3718	0.114*
N3	0.46595 (11)	0.82054 (17)	0.56868 (13)	0.056 (4)
H3A	0.4608	0.8449	0.5102	0.044*
H3B	0.4505	0.8821	0.6050	0.044*
H3C	0.4344	0.7541	0.5766	0.044*
O2W	0.5000	0.522 (3)	0.2500	0.068 (6)
H2W	0.532 (7)	0.453 (12)	0.281 (10)	0.04 (5)*
C1	0.5893 (11)	0.680 (2)	0.4426 (13)	0.040 (4)
C4	0.6031 (9)	0.8995 (17)	0.5728 (11)	0.037 (4)
C11	0.7035 (12)	0.3127 (17)	0.3105 (12)	0.032 (4)
C14	0.8185 (12)	0.1178 (17)	0.3993 (12)	0.041 (5)
C12	0.7419 (9)	0.2078 (14)	0.2567 (11)	0.036 (4)
H12A	0.7511	0.2382	0.1945	0.043*
H12B	0.7025	0.1387	0.2507	0.043*
C13	0.8236 (9)	0.1573 (15)	0.2992 (10)	0.038 (4)
H13	0.8391	0.0833	0.2634	0.046*
C3	0.5487 (9)	0.7862 (15)	0.5913 (11)	0.039 (4)
H3	0.5520	0.7725	0.6587	0.046*
C2	0.5752 (9)	0.6650 (14)	0.5470 (9)	0.033 (4)
H2A	0.5327	0.6014	0.5547	0.039*
H2B	0.6262	0.6355	0.5789	0.039*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0339 (17)	0.039 (3)	0.0257 (19)	0.0022 (8)	−0.0029 (15)	0.0001 (7)
O4	0.037 (9)	0.045 (15)	0.042 (11)	−0.010 (4)	0.012 (9)	0.001 (4)
O2	0.032 (5)	0.036 (7)	0.029 (6)	0.007 (4)	−0.003 (5)	0.003 (4)
O1	0.035 (8)	0.054 (14)	0.037 (10)	0.012 (5)	−0.003 (8)	−0.003 (4)
O14	0.055 (10)	0.072 (15)	0.031 (11)	−0.018 (6)	−0.005 (9)	0.016 (5)
O11	0.030 (10)	0.062 (17)	0.060 (13)	0.003 (5)	−0.002 (11)	−0.023 (6)
O13	0.075 (13)	0.040 (19)	0.046 (15)	−0.016 (7)	0.019 (13)	0.003 (5)
O12	0.040 (9)	0.063 (15)	0.041 (11)	0.007 (5)	−0.012 (9)	0.000 (5)
O3	0.036 (9)	0.033 (17)	0.067 (13)	−0.004 (5)	0.008 (10)	0.002 (5)
N13	0.025 (9)	0.062 (16)	0.023 (12)	0.004 (5)	0.001 (9)	0.001 (6)
O1W	0.106 (14)	0.046 (19)	0.081 (15)	−0.015 (7)	0.049 (13)	−0.014 (6)
N3	0.043 (12)	0.06 (2)	0.072 (16)	−0.009 (7)	0.022 (13)	−0.009 (7)
O2W	0.061 (8)	0.067 (9)	0.073 (9)	0.000	−0.004 (7)	0.000
C1	0.038 (5)	0.039 (6)	0.042 (6)	0.001 (4)	0.002 (4)	0.002 (4)
C4	0.040 (5)	0.036 (6)	0.035 (5)	−0.001 (4)	0.003 (4)	−0.003 (4)
C11	0.035 (5)	0.031 (6)	0.030 (5)	0.003 (4)	0.000 (4)	0.000 (4)
C14	0.051 (15)	0.05 (2)	0.026 (17)	0.003 (9)	0.005 (15)	−0.010 (8)
C12	0.034 (12)	0.032 (19)	0.041 (15)	0.010 (7)	0.001 (12)	0.001 (6)
C13	0.050 (13)	0.03 (2)	0.031 (15)	−0.013 (7)	−0.001 (13)	0.005 (6)
C3	0.034 (12)	0.05 (2)	0.034 (15)	−0.004 (7)	0.004 (12)	0.002 (7)
C2	0.043 (11)	0.038 (19)	0.017 (14)	−0.008 (7)	0.001 (11)	0.003 (6)

Geometric parameters (Å, º)

Zn1—O4^i	1.956 (9)	N3—H3A	0.8900
Zn1—O1	1.926 (10)	N3—H3B	0.8900
Zn1—O14^ii	1.977 (10)	N3—H3C	0.8900
Zn1—O11	1.942 (10)	N3—C3	1.402 (15)
O4—C4	1.282 (16)	O2W—H2W	0.99 (5)
O2—C1	1.25 (2)	C1—C2	1.54 (2)
O1—C1	1.256 (19)	C4—C3	1.52 (2)
O14—C14	1.310 (19)	C11—C12	1.51 (2)
O11—C11	1.27 (2)	C14—C13	1.51 (2)
O13—C14	1.218 (19)	C12—H12A	0.9700
O12—C11	1.23 (2)	C12—H12B	0.9700
O3—C4	1.217 (17)	C12—C13	1.52 (2)
N13—H13A	0.8900	C13—H13	0.9800
N13—H13B	0.8900	C3—H3	0.9800
N13—H13C	0.8900	C3—C2	1.508 (19)
N13—C13	1.499 (18)	C2—H2A	0.9700
O1W—H1WA	0.8396	C2—H2B	0.9700
O1W—H1WB	0.8415
O4^i—Zn1—O14^ii	99.7 (4)	O12—C11—O11	126.2 (17)
O1—Zn1—O4^i	100.2 (4)	O12—C11—C12	119.4 (15)
O1—Zn1—O14^ii	120.9 (4)	O14—C14—C13	115.4 (16)
O1—Zn1—O11	109.9 (6)	O13—C14—O14	122.0 (16)
O11—Zn1—O4^i	106.3 (4)	O13—C14—C13	122.3 (16)
O11—Zn1—O14^ii	116.6 (6)	C11—C12—H12A	108.5
C4—O4—Zn1^i	123.9 (11)	C11—C12—H12B	108.5
C1—O1—Zn1	135.1 (12)	C11—C12—C13	115.1 (16)
C14—O14—Zn1^ii	107.8 (11)	H12A—C12—H12B	107.5
C11—O11—Zn1	127.9 (11)	C13—C12—H12A	108.5
H13A—N13—H13B	109.5	C13—C12—H12B	108.5
H13A—N13—H13C	109.5	N13—C13—C14	108.7 (13)
H13B—N13—H13C	109.5	N13—C13—C12	110.8 (12)
C13—N13—H13A	109.5	N13—C13—H13	108.1
C13—N13—H13B	109.5	C14—C13—C12	113.1 (12)
C13—N13—H13C	109.5	C14—C13—H13	108.1
H1WA—O1W—H1WB	104.6	C12—C13—H13	108.1
H3A—N3—H3B	109.5	N3—C3—C4	108.2 (13)
H3A—N3—H3C	109.5	N3—C3—H3	105.0
H3B—N3—H3C	109.5	N3—C3—C2	114.3 (12)
C3—N3—H3A	109.5	C4—C3—H3	106.9
C3—N3—H3B	111.00	C2—C3—C4	114.9 (11)
C3—N3—H3C	108.00	C2—C3—H3	106.9
O2—C1—O1	123.1 (17)	C1—C2—H2A	109.1
O2—C1—C2	118.0 (16)	C1—C2—H2B	109.1
O1—C1—C2	118.8 (15)	C3—C2—C1	112.6 (13)
O4—C4—C3	114.5 (15)	C3—C2—H2A	109.1
O3—C4—O4	125.7 (14)	C3—C2—H2B	109.1
O3—C4—C3	119.7 (13)	H2A—C2—H2B	107.8
O11—C11—C12	114.3 (17)
Zn1—O1—C1—C2	−21 (3)	N3—C3—C4—O3	33.0 (19)
Zn1—O11—C11—C12	−171.6 (10)	C1—C2—C3—N3	74.0 (17)
O2—C1—C2—C3	−30 (3)	C1—C2—C3—C4	−50.4 (19)
O12—C11—C12—C13	−157.6 (15)	C11—C12—C13—N13	−69.0 (15)
N13—C13—C14—O13	−14 (2)	C11—C12—C13—C14	53.3 (18)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1.

(Zn-aspartate_sesquihydrate_0_85GPa)

Crystal data

C16H24N4O16Zn2·3(H2O)	F(000) = 1464
Mr = 713.18	Dx = 1.950 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 16.027 (2) Å	Cell parameters from 366 reflections
b = 10.5656 (8) Å	θ = 4.8–27.1°
c = 14.3681 (11) Å	µ = 2.08 mm^−1
β = 93.12 (2)°	T = 296 K
V = 2429.5 (4) Å^3	Plate, colourless
Z = 4	0.20 × 0.15 × 0.05 mm

Data collection

Multiwire proportional diffractometer	366 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.089
Graphite monochromator	θmax = 27.1°, θmin = 4.8°
ω scan	h = −3→3
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −13→13
Tmin = 0.695, Tmax = 0.901	l = −18→18
5840 measured reflections	12 standard reflections every 84 reflections
549 independent reflections	intensity decay: none

Refinement

Refinement on F^2	Hydrogen site location: mixed
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F^2 > 2σ(F^2)] = 0.042	w = 1/[σ^2(Fo^2) + (0.P)^2 + 18.3211P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.074	(Δ/σ)max < 0.001
S = 1.14	Δρmax = 0.19 e Å^−3
549 reflections	Δρmin = −0.19 e Å^−3
196 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
114 restraints	Extinction coefficient: 0.0024 (5)
Primary atom site location: dual

Special details

Experimental. Data were collected at room temperature and pressure of 0.85 (2) GPa (850000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7327 (3)	0.50538 (10)	0.45152 (7)	0.036 (5)
O4	0.6821 (19)	0.8699 (8)	0.5530 (6)	0.047 (3)
O2	0.5444 (13)	0.7613 (5)	0.3993 (4)	0.04 (2)
O1	0.6397 (18)	0.6085 (6)	0.4065 (4)	0.038 (3)
O14	0.7556 (16)	0.0454 (8)	0.4167 (5)	0.049 (3)
O11	0.7568 (15)	0.3774 (6)	0.3617 (5)	0.055 (3)
O13	0.8715 (16)	0.1431 (7)	0.4586 (5)	0.045 (4)
O12	0.625 (2)	0.3358 (10)	0.2995 (7)	0.056 (6)
O3	0.5716 (17)	1.0069 (6)	0.5838 (5)	0.046 (4)
N13	0.894 (2)	0.2494 (8)	0.2930 (6)	0.06 (3)
H13A	0.9092	0.2550	0.2345	0.069*
H13B	0.9368	0.2215	0.3293	0.069*
H13C	0.8784	0.3254	0.3125	0.069*
O1W	0.6011 (16)	0.9878 (12)	0.3254 (8)	0.068 (3)
H1WA	0.6515	0.9969	0.3427	0.103*
H1WB	0.5821	0.9390	0.3650	0.103*
N3	0.464 (2)	0.8206 (10)	0.5688 (7)	0.046 (5)
H3A	0.4584	0.8274	0.5070	0.055*
H3B	0.4526	0.8944	0.5947	0.055*
H3C	0.4299	0.7614	0.5882	0.055*
O2W	0.5000	0.5215 (14)	0.2500	0.071 (6)
H2W	0.541 (9)	0.475 (11)	0.269 (13)	0.12 (8)*
C1	0.587 (2)	0.6796 (9)	0.4430 (6)	0.025 (3)
C4	0.610 (2)	0.8989 (12)	0.5731 (8)	0.027 (4)
C11	0.702 (2)	0.3159 (16)	0.3068 (10)	0.037 (5)
C14	0.814 (2)	0.1161 (10)	0.4010 (8)	0.06 (4)
C12	0.738 (3)	0.2085 (10)	0.2541 (7)	0.041 (4)
H12A	0.7458	0.2360	0.1909	0.049*
H12B	0.6972	0.1400	0.2509	0.049*
C13	0.821 (2)	0.1577 (9)	0.2974 (6)	0.031 (3)
H13	0.8355	0.0822	0.2621	0.037*
C3	0.549 (2)	0.7858 (10)	0.5952 (9)	0.039 (4)
H3	0.5534	0.7710	0.6627	0.047*
C2	0.5734 (19)	0.6651 (8)	0.5472 (5)	0.031 (3)
H2A	0.5299	0.6027	0.5549	0.038*
H2B	0.6244	0.6328	0.5779	0.038*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.040 (14)	0.0317 (7)	0.0346 (7)	−0.0015 (17)	−0.0026 (16)	−0.0010 (5)
O4	0.047 (6)	0.045 (4)	0.050 (4)	−0.001 (4)	0.003 (4)	−0.006 (3)
O2	0.05 (7)	0.033 (4)	0.040 (4)	0.008 (8)	−0.014 (9)	0.003 (3)
O1	0.038 (6)	0.038 (3)	0.038 (3)	0.003 (4)	−0.001 (4)	0.000 (3)
O14	0.049 (6)	0.049 (3)	0.049 (4)	0.000 (4)	0.001 (4)	0.007 (3)
O11	0.054 (6)	0.054 (3)	0.057 (3)	0.000 (4)	0.002 (4)	−0.009 (3)
O13	0.044 (11)	0.054 (4)	0.036 (4)	0.000 (7)	0.000 (7)	0.005 (3)
O12	0.056 (12)	0.053 (6)	0.060 (6)	0.000 (8)	0.006 (8)	−0.008 (4)
O3	0.044 (11)	0.036 (4)	0.058 (4)	0.003 (7)	0.007 (7)	−0.002 (3)
N13	0.09 (9)	0.042 (5)	0.039 (5)	0.011 (15)	0.027 (12)	0.011 (4)
O1W	0.069 (4)	0.066 (3)	0.071 (3)	0.000 (2)	0.005 (2)	−0.001 (2)
N3	0.048 (11)	0.046 (5)	0.044 (5)	0.002 (8)	−0.003 (8)	−0.006 (4)
O2W	0.070 (12)	0.057 (7)	0.087 (8)	0.000	−0.006 (8)	0.000
C1	0.025 (6)	0.022 (3)	0.028 (4)	0.000 (4)	0.002 (4)	−0.006 (3)
C4	0.027 (4)	0.027 (4)	0.027 (4)	−0.0002 (11)	0.0014 (11)	−0.0002 (11)
C11	0.036 (8)	0.037 (6)	0.036 (6)	−0.001 (4)	0.001 (4)	0.000 (4)
C14	0.12 (12)	0.021 (6)	0.034 (7)	0.002 (14)	0.010 (16)	0.004 (5)
C12	0.041 (6)	0.040 (4)	0.042 (4)	0.001 (4)	0.002 (4)	−0.002 (4)
C13	0.031 (6)	0.032 (4)	0.030 (4)	0.001 (4)	0.003 (4)	0.001 (3)
C3	0.039 (7)	0.036 (5)	0.042 (5)	−0.001 (4)	0.001 (4)	0.003 (3)
C2	0.031 (6)	0.032 (4)	0.031 (4)	0.001 (4)	0.002 (4)	−0.001 (3)

Geometric parameters (Å, º)

Zn1—O4^i	1.90 (2)	O1W—H1WB	0.8377
Zn1—O11	1.922 (9)	N3—C3	1.44 (4)
Zn1—O1	1.93 (2)	N3—H3A	0.8900
Zn1—O14^ii	1.967 (8)	N3—H3B	0.8900
O4—C4	1.25 (4)	N3—H3C	0.8900
O4—Zn1^i	1.90 (2)	O2W—H2W	0.85 (5)
O2—C1	1.25 (2)	C1—C2	1.533 (14)
O1—C1	1.27 (3)	C4—C3	1.58 (4)
O14—C14	1.22 (3)	C11—C12	1.49 (3)
O14—Zn1^ii	1.967 (8)	C14—C13	1.563 (14)
O11—C11	1.32 (3)	C12—C13	1.54 (5)
O13—C14	1.24 (3)	C12—H12A	0.9700
O12—C11	1.26 (4)	C12—H12B	0.9700
O3—C4	1.31 (2)	C13—H13	0.9800
N13—C13	1.52 (4)	C3—C2	1.509 (17)
N13—H13A	0.8900	C3—H3	0.9800
N13—H13B	0.8900	C2—H2A	0.9700
N13—H13C	0.8900	C2—H2B	0.9700
O1W—H1WA	0.8366
O4^i—Zn1—O11	107.1 (8)	O12—C11—C12	119 (3)
O4^i—Zn1—O1	98.1 (8)	O11—C11—C12	115 (3)
O11—Zn1—O1	110.6 (6)	O14—C14—O13	124.4 (13)
O4^i—Zn1—O14^ii	101.0 (7)	O14—C14—C13	117 (2)
O11—Zn1—O14^ii	116.3 (4)	O13—C14—C13	118 (3)
O1—Zn1—O14^ii	120.5 (7)	C11—C12—C13	113.8 (19)
C4—O4—Zn1^i	121.0 (11)	C11—C12—H12A	108.8
C1—O1—Zn1	135.9 (9)	C13—C12—H12A	108.8
C14—O14—Zn1^ii	108.1 (13)	C11—C12—H12B	108.8
C11—O11—Zn1	127 (2)	C13—C12—H12B	108.8
C13—N13—H13A	109.5	H12A—C12—H12B	107.7
C13—N13—H13B	109.5	N13—C13—C12	114.4 (13)
H13A—N13—H13B	109.5	N13—C13—C14	108.6 (18)
C13—N13—H13C	109.5	C12—C13—C14	112 (3)
H13A—N13—H13C	109.5	N13—C13—H13	107.2
H13B—N13—H13C	109.5	C12—C13—H13	107.2
H1WA—O1W—H1WB	104.4	C14—C13—H13	107.2
C3—N3—H3A	109.5	N3—C3—C2	110.8 (19)
C3—N3—H3B	109.5	N3—C3—C4	109.5 (16)
H3A—N3—H3B	109.5	C2—C3—C4	112 (2)
C3—N3—H3C	109.5	N3—C3—H3	108.2
H3A—N3—H3C	109.5	C2—C3—H3	108.2
H3B—N3—H3C	109.5	C4—C3—H3	108.2
O2—C1—O1	124.1 (11)	C3—C2—C1	114.6 (8)
O2—C1—C2	117 (2)	C3—C2—H2A	108.6
O1—C1—C2	118.6 (15)	C1—C2—H2A	108.6
O4—C4—O3	133 (2)	C3—C2—H2B	108.6
O4—C4—C3	116.6 (16)	C1—C2—H2B	108.6
O3—C4—C3	110 (3)	H2A—C2—H2B	107.6
O12—C11—O11	126 (2)
C1—C2—C3—N3	73 (3)	C11—C12—C13—C14	56 (2)
C1—C2—C3—C4	−50 (3)	N13—C13—C14—O13	−11 (2)
N3—C3—C4—O3	32.7 (15)	O12—C11—C12—C13	−155 (2)
O2—C1—C2—C3	−31 (3)	Zn1—O1—C1—C2	−18 (3)
C11—C12—C13—N13	−68 (2)	Zn1—O11—C11—C12	−171.4 (9)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1.

(Zn-aspartate_sesquihydrate_1_15GPa)

Crystal data

C16H24N4O16Zn2·3(H2O)	F(000) = 1464
Mr = 713.18	Dx = 1.985 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 16.005 (3) Å	Cell parameters from 332 reflections
b = 10.4707 (8) Å	θ = 0.7–0.9°
c = 14.2629 (10) Å	µ = 2.12 mm^−1
β = 93.08 (3)°	T = 296 K
V = 2386.8 (5) Å^3	Plate, colourless
Z = 4	0.20 × 0.15 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.070
Radiation source: sealed x-ray tube	θmax = 27.0°, θmin = 3.7°
ω scan	h = −3→3
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −12→13
Tmin = 3.74, Tmax = 27.015	l = −18→17
4732 measured reflections	12 standard reflections every 84 reflections
436 independent reflections	intensity decay: none
332 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.031	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.077	w = 1/[σ^2(Fo^2) + (0.0394P)^2 + 10.5512P] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max < 0.001
436 reflections	Δρmax = 0.16 e Å^−3
196 parameters	Δρmin = −0.14 e Å^−3
134 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 1.15 (2) GPa (1150000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7342 (4)	0.50578 (9)	0.45238 (7)	0.031 (2)
O4	0.681 (3)	0.8672 (9)	0.5518 (7)	0.043 (4)
O2	0.5417 (16)	0.7615 (6)	0.3992 (4)	0.034 (5)
O1	0.641 (3)	0.6084 (7)	0.4066 (5)	0.036 (3)
O14	0.752 (2)	0.0453 (8)	0.4140 (5)	0.050 (3)
O11	0.755 (2)	0.3781 (7)	0.3600 (5)	0.051 (3)
O13	0.869 (2)	0.1410 (7)	0.4583 (5)	0.044 (5)
O12	0.628 (3)	0.3387 (12)	0.2978 (9)	0.055 (6)
O3	0.570 (2)	1.0080 (6)	0.5850 (5)	0.044 (5)
N13	0.890 (2)	0.2487 (7)	0.2914 (5)	0.035 (5)
H13A	0.902048	0.260648	0.231680	0.042*
H13B	0.935479	0.218320	0.323216	0.042*
H13C	0.875645	0.322745	0.316286	0.042*
O1W	0.600 (2)	0.9877 (11)	0.3208 (6)	0.065 (5)
H1WA	0.647946	0.986475	0.349458	0.097*
H1WB	0.571482	0.932492	0.349269	0.097*
N3	0.463 (3)	0.8190 (11)	0.5690 (7)	0.044 (5)
H3A	0.458011	0.829716	0.507056	0.053*
H3B	0.450015	0.891253	0.597471	0.053*
H3C	0.429201	0.756877	0.585829	0.053*
O2W	0.500000	0.5222 (15)	0.250000	0.065 (6)
H2W	0.557846	0.486394	0.253083	0.16 (10)*
C1	0.583 (3)	0.6792 (10)	0.4439 (7)	0.029 (3)
C4	0.607 (5)	0.9000 (12)	0.5722 (9)	0.023 (4)
C11	0.697 (4)	0.3184 (17)	0.3063 (12)	0.029 (5)
C14	0.814 (3)	0.1144 (10)	0.3988 (8)	0.030 (4)
C12	0.739 (4)	0.2082 (10)	0.2522 (8)	0.037 (4)
H12A	0.699387	0.138367	0.245108	0.044*
H12B	0.749627	0.238699	0.189713	0.044*
C13	0.820 (3)	0.1557 (9)	0.2963 (7)	0.029 (3)
H13	0.835105	0.079955	0.260390	0.035*
C3	0.548 (3)	0.7853 (11)	0.5958 (9)	0.037 (5)
H3	0.552212	0.771523	0.663808	0.045*
C2	0.573 (2)	0.6632 (8)	0.5485 (6)	0.029 (3)
H2A	0.530070	0.599040	0.557809	0.035*
H2B	0.624761	0.632569	0.578007	0.035*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.034 (6)	0.0293 (7)	0.0294 (7)	0.0005 (18)	−0.0040 (17)	−0.0008 (5)
O4	0.043 (7)	0.038 (4)	0.048 (4)	−0.003 (5)	0.002 (5)	−0.005 (3)
O2	0.034 (13)	0.033 (3)	0.035 (3)	0.001 (7)	−0.010 (7)	0.005 (3)
O1	0.036 (7)	0.038 (3)	0.034 (3)	0.001 (5)	0.000 (5)	−0.001 (3)
O14	0.050 (7)	0.053 (4)	0.048 (4)	0.000 (5)	0.004 (5)	0.007 (3)
O11	0.051 (7)	0.048 (3)	0.055 (4)	0.000 (5)	0.003 (5)	−0.020 (3)
O13	0.043 (13)	0.053 (4)	0.036 (4)	−0.003 (9)	0.006 (9)	0.002 (3)
O12	0.054 (14)	0.056 (7)	0.054 (6)	−0.003 (10)	−0.001 (10)	−0.004 (4)
O3	0.044 (13)	0.036 (4)	0.054 (4)	0.005 (8)	0.010 (9)	0.001 (3)
N13	0.035 (13)	0.038 (4)	0.034 (4)	−0.001 (9)	0.016 (9)	0.007 (4)
O1W	0.066 (13)	0.050 (4)	0.081 (6)	−0.001 (8)	0.022 (9)	−0.010 (4)
N3	0.045 (13)	0.043 (6)	0.043 (5)	0.000 (10)	0.006 (9)	−0.004 (4)
O2W	0.063 (14)	0.049 (6)	0.084 (8)	0.000	−0.001 (10)	0.000
C1	0.029 (7)	0.031 (4)	0.027 (4)	−0.001 (5)	0.001 (5)	−0.001 (3)
C4	0.023 (7)	0.023 (5)	0.025 (4)	−0.001 (5)	0.003 (5)	0.001 (4)
C11	0.028 (8)	0.028 (6)	0.029 (6)	0.001 (5)	0.001 (5)	−0.002 (4)
C14	0.030 (7)	0.027 (4)	0.034 (4)	0.000 (5)	0.001 (5)	0.000 (4)
C12	0.037 (7)	0.039 (4)	0.035 (4)	0.001 (5)	0.003 (5)	0.000 (4)
C13	0.029 (7)	0.030 (4)	0.029 (4)	0.002 (5)	0.003 (5)	−0.001 (3)
C3	0.037 (8)	0.038 (5)	0.037 (5)	−0.001 (5)	0.002 (5)	0.001 (4)
C2	0.029 (7)	0.028 (4)	0.031 (4)	0.002 (5)	0.001 (5)	0.001 (3)

Geometric parameters (Å, º)

Zn1—O4^i	1.90 (4)	N3—H3A	0.8900
Zn1—O1	1.92 (4)	N3—H3B	0.8900
Zn1—O14^ii	1.981 (8)	N3—H3C	0.8900
Zn1—O11	1.918 (9)	N3—C3	1.43 (5)
O4—C4	1.28 (9)	O2W—H2W	0.9976
O2—C1	1.24 (3)	C1—C2	1.518 (16)
O1—C1	1.32 (5)	C4—C3	1.58 (6)
O14—C14	1.26 (5)	C11—C12	1.56 (4)
O11—C11	1.33 (4)	C14—C13	1.534 (15)
O13—C14	1.23 (5)	C12—H12A	0.9700
O12—C11	1.13 (9)	C12—H12B	0.9700
O3—C4	1.29 (4)	C12—C13	1.52 (6)
N13—H13A	0.8900	C13—H13	0.9800
N13—H13B	0.8900	C3—H3	0.9800
N13—H13C	0.8900	C3—C2	1.51 (2)
N13—C13	1.49 (4)	C2—H2A	0.9700
O1W—H1WA	0.8521	C2—H2B	0.9600
O1W—H1WB	0.8511
O4^i—Zn1—O1	98.0 (14)	O12—C11—O11	129 (2)
O4^i—Zn1—O14^ii	100.0 (9)	O12—C11—C12	122 (3)
O4^i—Zn1—O11	108.5 (11)	O14—C14—C13	115 (3)
O1—Zn1—O14^ii	121.7 (9)	O13—C14—O14	124.2 (15)
O11—Zn1—O1	108.4 (8)	O13—C14—C13	121 (4)
O11—Zn1—O14^ii	117.2 (4)	C11—C12—H12A	108.2
C4—O4—Zn1^i	119.2 (14)	C11—C12—H12B	108.2
C1—O1—Zn1	136.4 (11)	H12A—C12—H12B	107.3
C14—O14—Zn1^ii	105.6 (17)	C13—C12—C11	116 (2)
C11—O11—Zn1	126 (2)	C13—C12—H12A	108.2
H13A—N13—H13B	109.5	C13—C12—H12B	108.2
H13A—N13—H13C	109.5	N13—C13—C14	109 (2)
H13B—N13—H13C	109.5	N13—C13—C12	112.0 (16)
C13—N13—H13A	109.5	N13—C13—H13	107.5
C13—N13—H13B	109.5	C14—C13—H13	107.5
C13—N13—H13C	109.5	C12—C13—C14	113 (3)
H1WA—O1W—H1WB	104.6	C12—C13—H13	107.5
H3A—N3—H3B	109.5	N3—C3—C4	109 (3)
H3A—N3—H3C	109.5	N3—C3—H3	108.2
H3B—N3—H3C	109.5	N3—C3—C2	111 (2)
C3—N3—H3A	109.5	C4—C3—H3	108.2
C3—N3—H3B	109.5	C2—C3—C4	112 (3)
C3—N3—H3C	109.5	C2—C3—H3	108.2
O2—C1—O1	123.2 (14)	C1—C2—H2A	109.0
O2—C1—C2	120 (3)	C1—C2—H2B	109.0
O1—C1—C2	117 (2)	C3—C2—C1	113.0 (10)
O4—C4—O3	135 (4)	C3—C2—H2A	109.0
O4—C4—C3	115 (2)	C3—C2—H2B	109.0
O3—C4—C3	111 (5)	H2A—C2—H2B	107.8
O11—C11—C12	109 (4)
Zn1—O1—C1—C2	−14 (5)	N3—C3—C4—O3	35 (2)
Zn1—O11—C11—C12	−171.5 (10)	C1—C2—C3—N3	71 (4)
O2—C1—C2—C3	−29 (5)	C1—C2—C3—C4	−51 (4)
O12—C11—C12—C13	−156 (3)	C11—C12—C13—N13	−70 (3)
N13—C13—C14—O13	−12 (3)	C11—C12—C13—C14	53 (3)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1.

(Zn-aspartate_sesquihydrate_1_44GPa)

Crystal data

C16H24N4O16Zn2·3(H2O)	F(000) = 1464
Mr = 713.18	Dx = 1.992 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 15.950 (3) Å	Cell parameters from 333 reflections
b = 10.4707 (8) Å	θ = 3.7–27.0°
c = 14.2629 (10) Å	µ = 2.12 mm^−1
β = 93.08 (3)°	T = 296 K
V = 2378.6 (5) Å^3	Plate, colourless
Z = 4	0.20 × 0.15 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.063
Radiation source: sealed x-ray tube	θmax = 27.0°, θmin = 3.7°
ω scan	h = −3→3
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −12→13
Tmin = 0.689, Tmax = 0.899	l = −18→17
4750 measured reflections	12 standard reflections every 84 reflections
437 independent reflections	intensity decay: none
333 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.031	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.076	w = 1/[σ^2(Fo^2) + (0.0398P)^2 + 8.8556P] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max < 0.001
437 reflections	Δρmax = 0.16 e Å^−3
196 parameters	Δρmin = −0.14 e Å^−3
110 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 1.44 (2) GPa (1440000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7344 (3)	0.50578 (9)	0.45237 (7)	0.048 (7)
O4	0.680 (3)	0.8673 (10)	0.5517 (7)	0.043 (4)
O2	0.5414 (16)	0.7614 (6)	0.3991 (4)	0.035 (5)
O1	0.642 (3)	0.6084 (7)	0.4066 (5)	0.036 (3)
O14	0.751 (2)	0.0454 (8)	0.4140 (5)	0.051 (3)
O11	0.756 (2)	0.3780 (6)	0.3602 (5)	0.053 (3)
O13	0.870 (3)	0.1410 (7)	0.4583 (5)	0.043 (5)
O12	0.628 (3)	0.3390 (14)	0.2981 (9)	0.058 (7)
O3	0.571 (2)	1.0081 (6)	0.5856 (5)	0.044 (5)
N13	0.890 (2)	0.2491 (8)	0.2913 (5)	0.036 (5)
H13A	0.902011	0.261259	0.231597	0.043*
H13B	0.935850	0.219295	0.323109	0.043*
H13C	0.875233	0.322969	0.316229	0.043*
O1W	0.599 (2)	0.9876 (13)	0.3209 (8)	0.066 (5)
H1WA	0.647766	0.987709	0.345264	0.090*
H1WB	0.573520	0.935027	0.352538	0.090*
N3	0.462 (3)	0.8194 (12)	0.5692 (7)	0.044 (5)
H3A	0.455852	0.832236	0.507521	0.053*
H3B	0.447851	0.890281	0.599169	0.053*
H3C	0.4344	0.7541	0.5766	0.044*
O2W	0.500000	0.5222 (15)	0.250000	0.066 (7)
H2W	0.558 (6)	0.487 (11)	0.250 (14)	0.09 (9)*
C1	0.584 (4)	0.6789 (10)	0.4439 (7)	0.05 (7)
C4	0.607 (5)	0.9002 (12)	0.5722 (9)	0.023 (4)
C11	0.695 (5)	0.3182 (18)	0.3057 (12)	0.028 (5)
C14	0.816 (4)	0.1146 (10)	0.3990 (8)	0.031 (4)
C12	0.738 (4)	0.2086 (11)	0.2521 (8)	0.037 (4)
H12A	0.698754	0.138268	0.245150	0.045*
H12B	0.748473	0.239142	0.189566	0.045*
C13	0.821 (3)	0.1561 (9)	0.2963 (7)	0.03 (4)
H13	0.836265	0.080663	0.260080	0.039*
C3	0.550 (4)	0.7854 (11)	0.5956 (9)	0.038 (5)
H3	0.554825	0.771707	0.663670	0.046*
C2	0.573 (2)	0.6631 (7)	0.5486 (5)	0.029 (3)
H2A	0.529403	0.600307	0.557710	0.035*
H2B	0.624838	0.630823	0.578302	0.035*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.08 (2)	0.0293 (7)	0.0292 (7)	0.0005 (19)	−0.0037 (18)	−0.0008 (5)
O4	0.043 (7)	0.038 (4)	0.049 (5)	−0.003 (5)	0.002 (5)	−0.006 (3)
O2	0.035 (13)	0.034 (3)	0.035 (3)	0.000 (7)	−0.010 (7)	0.006 (3)
O1	0.036 (7)	0.038 (3)	0.034 (3)	0.002 (5)	−0.001 (5)	−0.002 (3)
O14	0.051 (7)	0.054 (4)	0.048 (4)	0.000 (5)	0.005 (5)	0.007 (3)
O11	0.053 (7)	0.050 (3)	0.056 (4)	−0.001 (5)	0.002 (5)	−0.020 (3)
O13	0.042 (13)	0.052 (4)	0.036 (4)	−0.001 (9)	0.005 (9)	0.001 (3)
O12	0.058 (14)	0.059 (7)	0.058 (7)	−0.003 (10)	0.000 (10)	−0.004 (5)
O3	0.044 (13)	0.039 (4)	0.050 (4)	0.007 (8)	0.013 (9)	−0.001 (3)
N13	0.036 (13)	0.036 (4)	0.036 (4)	−0.001 (9)	0.016 (9)	0.008 (4)
O1W	0.067 (13)	0.050 (4)	0.083 (6)	−0.002 (8)	0.020 (9)	−0.010 (4)
N3	0.046 (13)	0.043 (5)	0.045 (5)	0.000 (10)	0.006 (9)	−0.005 (5)
O2W	0.064 (14)	0.048 (6)	0.086 (8)	0.000	−0.001 (10)	0.000
C1	0.1 (2)	0.034 (6)	0.025 (5)	−0.02 (2)	0.01 (2)	−0.003 (4)
C4	0.023 (7)	0.022 (5)	0.025 (4)	−0.002 (5)	0.002 (5)	0.001 (4)
C11	0.028 (8)	0.028 (5)	0.029 (6)	0.001 (5)	0.002 (5)	−0.002 (4)
C14	0.031 (7)	0.027 (4)	0.034 (4)	0.000 (5)	0.001 (5)	0.000 (4)
C12	0.037 (7)	0.038 (4)	0.037 (4)	0.000 (5)	0.003 (5)	0.000 (4)
C13	0.04 (12)	0.032 (5)	0.029 (5)	0.021 (17)	0.009 (16)	−0.001 (4)
C3	0.038 (8)	0.038 (5)	0.038 (5)	−0.001 (5)	0.002 (5)	0.000 (4)
C2	0.028 (7)	0.027 (3)	0.031 (4)	0.003 (5)	0.002 (5)	0.002 (3)

Geometric parameters (Å, º)

Zn1—O4^i	1.91 (4)	N3—H3A	0.8900
Zn1—O1	1.91 (4)	N3—H3B	0.8900
Zn1—O14^ii	1.981 (8)	N3—H3C	0.8200
Zn1—O11	1.919 (9)	N3—C3	1.48 (8)
O4—C4	1.26 (9)	O2W—H2W	0.99 (6)
O2—C1	1.25 (3)	C1—C2	1.523 (16)
O1—C1	1.31 (5)	C4—C3	1.55 (6)
O14—C14	1.29 (5)	C11—C12	1.56 (5)
O11—C11	1.36 (5)	C14—C13	1.535 (15)
O13—C14	1.21 (5)	C12—H12A	0.9700
O12—C11	1.09 (11)	C12—H12B	0.9700
O3—C4	1.29 (4)	C12—C13	1.54 (6)
N13—H13A	0.8900	C13—H13	0.9800
N13—H13B	0.8900	C3—H3	0.9800
N13—H13C	0.8900	C3—C2	1.50 (2)
N13—C13	1.48 (4)	C2—H2A	0.9700
O1W—H1WA	0.8323	C2—H2B	0.9700
O1W—H1WB	0.8325
O4^i—Zn1—O1	98.1 (14)	O12—C11—O11	129 (3)
O4^i—Zn1—O14^ii	99.8 (9)	O12—C11—C12	124 (4)
O4^i—Zn1—O11	108.1 (11)	O14—C14—C13	114 (3)
O1—Zn1—O14^ii	121.9 (9)	O13—C14—O14	124.2 (16)
O1—Zn1—O11	108.7 (8)	O13—C14—C13	122 (4)
O11—Zn1—O14^ii	117.0 (4)	C11—C12—H12A	108.0
C4—O4—Zn1^i	119.1 (16)	C11—C12—H12B	108.0
C1—O1—Zn1	136.3 (11)	H12A—C12—H12B	107.3
C14—O14—Zn1^ii	105.0 (16)	C13—C12—C11	117 (3)
C11—O11—Zn1	124 (3)	C13—C12—H12A	108.0
H13A—N13—H13B	109.5	C13—C12—H12B	108.0
H13A—N13—H13C	109.5	N13—C13—C14	108 (3)
H13B—N13—H13C	109.5	N13—C13—C12	112.0 (16)
C13—N13—H13A	109.5	N13—C13—H13	107.6
C13—N13—H13B	109.5	C14—C13—C12	114 (3)
C13—N13—H13C	109.5	C14—C13—H13	107.6
H1WA—O1W—H1WB	104.4	C12—C13—H13	107.6
H3A—N3—H3B	109.5	N3—C3—C4	109 (3)
H3A—N3—H3C	103.0	N3—C3—H3	108.1
H3B—N3—H3C	119.0	N3—C3—C2	110 (3)
C3—N3—H3A	109.5	C4—C3—H3	108.1
C3—N3—H3B	109.5	C2—C3—C4	114 (4)
C3—N3—H3C	106.0	C2—C3—H3	108.1
O2—C1—O1	123.6 (14)	C1—C2—H2A	109.0
O2—C1—C2	119 (3)	C1—C2—H2B	109.0
O1—C1—C2	117 (2)	C3—C2—C1	112.9 (10)
O4—C4—O3	135 (5)	C3—C2—H2A	109.0
O4—C4—C3	113 (2)	C3—C2—H2B	109.0
O3—C4—C3	112 (5)	H2A—C2—H2B	107.8
O11—C11—C12	108 (5)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1.

(Zn-aspartate_sesquihydrate_1_62GPa)

Crystal data

C16H30N4O19Zn2	F(000) = 1464
Mr = 713.18	Dx = 1.999 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 15.916 (5) Å	Cell parameters from 316 reflections
b = 10.4593 (12) Å	θ = 3.8–27.0°
c = 14.2566 (15) Å	µ = 2.13 mm^−1
β = 93.09 (4)°	T = 296 K
V = 2369.9 (8) Å^3	Plate, colourless
Z = 4	0.20 × 0.15 × 0.15 mm

Data collection

Radiation source: fine-focus sealed tube	Rint = 0.101
Graphite monochromator	θmax = 27.0°, θmin = 3.8°
ω scan	h = −3→3
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −12→13
Tmin = 0.688, Tmax = 0.969	l = −18→17
4699 measured reflections	12 standard reflections every 84 reflections
433 independent reflections	intensity decay: none
316 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.039	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.099	w = 1/[σ^2(Fo^2) + (0.0636P)^2 + 0.3086P] where P = (Fo^2 + 2Fc^2)/3
S = 1.14	(Δ/σ)max < 0.001
433 reflections	Δρmax = 0.15 e Å^−3
196 parameters	Δρmin = −0.15 e Å^−3
138 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 1.62 (2) GPa (1620000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7346 (4)	0.50574 (9)	0.45275 (7)	0.050 (8)
O4	0.685 (3)	0.8658 (10)	0.5525 (8)	0.047 (6)
O2	0.5414 (15)	0.7599 (6)	0.3991 (4)	0.040 (9)
O1	0.641 (3)	0.6082 (7)	0.4068 (5)	0.042 (5)
O14	0.749 (2)	0.0450 (9)	0.4137 (5)	0.052 (5)
O11	0.7560 (19)	0.3781 (7)	0.3604 (5)	0.059 (5)
O13	0.867 (2)	0.1406 (7)	0.4584 (5)	0.043 (9)
O12	0.625 (2)	0.3381 (14)	0.2979 (11)	0.056 (10)
O3	0.568 (2)	1.0089 (6)	0.5857 (6)	0.048 (9)
N13	0.890 (3)	0.2486 (7)	0.2908 (5)	0.037 (4)
H13A	0.8944	0.2735	0.2315	0.045*
H13B	0.9381	0.2110	0.3110	0.045*
H13C	0.8809	0.3163	0.3265	0.045*
O1W	0.597 (3)	0.9887 (11)	0.3191 (7)	0.071 (5)
H1WB	0.5595	0.9411	0.3406	0.107*
H1WA	0.6410	0.9732	0.3541	0.107*
N3	0.463 (2)	0.8212 (11)	0.5690 (7)	0.042 (5)
H3A	0.4604	0.8383	0.5078	0.051*
H3B	0.4502	0.8910	0.6008	0.051*
H3C	0.4344	0.7541	0.5766	0.044*
O2W	0.5000	0.5233 (17)	0.2500	0.067 (6)
C1	0.580 (3)	0.6799 (11)	0.4446 (7)	0.034 (5)
C4	0.607 (3)	0.9015 (12)	0.5701 (10)	0.028 (6)
C11	0.702 (2)	0.321 (2)	0.3052 (16)	0.033 (7)
C14	0.810 (4)	0.1150 (12)	0.3972 (8)	0.034 (5)
C13	0.819 (3)	0.1562 (9)	0.2963 (7)	0.033 (5)
H13	0.8337	0.0799	0.2606	0.040*
C3	0.543 (2)	0.7830 (11)	0.5962 (9)	0.040 (6)
H3	0.5467	0.7702	0.6644	0.048*
C12	0.740 (3)	0.2090 (10)	0.2512 (8)	0.038 (5)
H12A	0.6990	0.1409	0.2448	0.046*
H12B	0.7517	0.2381	0.1886	0.046*
C2	0.573 (2)	0.6610 (7)	0.5488 (5)	0.032 (5)
H2A	0.6268	0.6356	0.5773	0.039*
H2B	0.5329	0.5928	0.5589	0.039*
H2W	0.549 (6)	0.486 (10)	0.251 (13)	0.10 (8)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.08 (2)	0.0331 (8)	0.0311 (8)	−0.0017 (19)	−0.005 (2)	−0.0008 (5)
O4	0.047 (14)	0.034 (5)	0.059 (6)	−0.011 (10)	0.001 (10)	−0.005 (4)
O2	0.04 (3)	0.038 (4)	0.040 (3)	0.000 (9)	−0.026 (9)	0.005 (3)
O1	0.042 (14)	0.044 (4)	0.038 (4)	0.000 (9)	−0.008 (9)	−0.004 (3)
O14	0.052 (14)	0.057 (4)	0.046 (4)	−0.009 (9)	−0.007 (9)	0.014 (4)
O11	0.061 (14)	0.052 (4)	0.066 (4)	−0.002 (8)	0.010 (9)	−0.023 (4)
O13	0.03 (3)	0.054 (4)	0.039 (4)	−0.016 (12)	−0.007 (12)	0.005 (3)
O12	0.05 (3)	0.070 (8)	0.052 (7)	−0.007 (16)	0.002 (16)	−0.015 (5)
O3	0.05 (3)	0.039 (4)	0.060 (4)	0.015 (10)	0.026 (14)	−0.006 (3)
N13	0.038 (10)	0.036 (4)	0.040 (4)	0.000 (8)	0.010 (7)	0.006 (3)
O1W	0.073 (11)	0.057 (5)	0.086 (5)	−0.003 (7)	0.023 (8)	−0.009 (4)
N3	0.043 (11)	0.040 (5)	0.045 (5)	0.008 (8)	0.007 (8)	0.002 (4)
O2W	0.065 (12)	0.050 (6)	0.087 (8)	0.000	−0.002 (9)	0.000
C1	0.036 (14)	0.036 (5)	0.031 (5)	−0.001 (10)	0.000 (10)	0.001 (4)
C4	0.027 (14)	0.022 (6)	0.035 (6)	0.001 (10)	0.012 (10)	0.003 (5)
C11	0.031 (15)	0.030 (7)	0.037 (8)	0.003 (11)	−0.001 (11)	0.007 (5)
C14	0.034 (14)	0.034 (6)	0.036 (5)	0.001 (10)	0.009 (10)	0.005 (5)
C13	0.033 (14)	0.036 (5)	0.032 (5)	0.003 (10)	0.008 (9)	−0.004 (4)
C3	0.042 (14)	0.040 (6)	0.040 (6)	−0.012 (10)	0.001 (10)	−0.001 (5)
C12	0.038 (14)	0.037 (5)	0.040 (5)	0.001 (10)	0.006 (10)	−0.004 (4)
C2	0.032 (14)	0.033 (4)	0.032 (4)	−0.004 (9)	−0.002 (9)	−0.001 (3)

Geometric parameters (Å, º)

Zn1—O4^i	1.85 (3)	O1W—H1WA	0.8502
Zn1—O11	1.919 (9)	N3—C3	1.371 (11)
Zn1—O1	1.92 (3)	N3—H3A	0.8900
Zn1—O14^ii	1.980 (8)	N3—H3B	0.8900
O4—C4	1.340 (11)	N3—H3C	0.8500
O4—Zn1^i	1.85 (3)	O2W—H2W	0.87 (5)
O2—C1	1.21 (3)	C1—C2	1.510 (14)
O1—C1	1.35 (4)	C4—C3	1.66 (4)
O14—C14	1.25 (5)	C11—C12	1.54 (4)
O14—Zn1^ii	1.980 (8)	C14—C13	1.516 (16)
O11—C11	1.28 (3)	C13—C12	1.48 (6)
O13—C14	1.25 (5)	C13—H13	0.9800
O12—C11	1.238 (11)	C3—C2	1.529 (19)
O3—C4	1.31 (3)	C3—H3	0.9800
N13—C13	1.49 (5)	C12—H12A	0.9700
N13—H13A	0.8900	C12—H12B	0.9700
N13—H13B	0.8900	C2—H2A	0.9700
N13—H13C	0.8900	C2—H2B	0.9700
O1W—H1WB	0.8500
O4^i—Zn1—O11	109.2 (10)	O12—C11—C12	119 (3)
O4^i—Zn1—O1	96.0 (10)	O11—C11—C12	113 (3)
O11—Zn1—O1	108.5 (8)	O13—C14—O14	122.3 (14)
O4^i—Zn1—O14^ii	100.3 (8)	O13—C14—C13	120 (4)
O11—Zn1—O14^ii	117.0 (5)	O14—C14—C13	117 (3)
O1—Zn1—O14^ii	122.4 (9)	C12—C13—N13	111.2 (16)
C4—O4—Zn1^i	117.0 (13)	C12—C13—C14	113 (3)
C1—O1—Zn1	136.7 (11)	N13—C13—C14	110 (3)
C14—O14—Zn1^ii	105.9 (17)	C12—C13—H13	107.3
C11—O11—Zn1	128 (2)	N13—C13—H13	107.3
C13—N13—H13A	109.5	C14—C13—H13	107.3
C13—N13—H13B	109.5	N3—C3—C2	114.8 (19)
H13A—N13—H13B	109.5	N3—C3—C4	106.8 (18)
C13—N13—H13C	109.5	C2—C3—C4	109 (2)
H13A—N13—H13C	109.5	N3—C3—H3	108.8
H13B—N13—H13C	109.5	C2—C3—H3	108.8
H1WB—O1W—H1WA	104.5	C4—C3—H3	108.8
C3—N3—H3A	109.5	C13—C12—C11	114.4 (18)
C3—N3—H3B	109.5	C13—C12—H12A	108.7
H3A—N3—H3B	109.5	C11—C12—H12A	108.7
C3—N3—H3C	103.0	C13—C12—H12B	108.7
H3A—N3—H3C	107.0	C11—C12—H12B	108.7
H3B—N3—H3C	118.0	H12A—C12—H12B	107.6
O2—C1—O1	121.6 (13)	C1—C2—C3	111.7 (10)
O2—C1—C2	123 (2)	C1—C2—H2A	109.3
O1—C1—C2	115 (2)	C3—C2—H2A	109.3
O3—C4—O4	136 (2)	C1—C2—H2B	109.3
O3—C4—C3	108 (3)	C3—C2—H2B	109.3
O4—C4—C3	115.0 (19)	H2A—C2—H2B	107.9
O12—C11—O11	128 (3)
C1—C2—C3—N3	66 (3)	N13—C13—C14—O13	−12 (3)
C1—C2—C3—C4	−54 (4)	O12—C11—C12—C13	−152 (3)
N3—C3—C4—O3	36.8 (14)	Zn1—O1—C1—C2	−13 (5)
O2—C1—C2—C3	−25 (5)	Zn1—O11—C11—C12	−170.9 (9)
C11—C12—C13—N13	−70 (2)	Zn1—O4^i—C4^i—C3^i	167.6 (10)
C11—C12—C13—C14	55 (3)	Zn1—O14^ii—C14^ii—C13^ii	−173.5 (19)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1.

(Zn-aspartate_sesquihydrate_1_82GPa)

Crystal data

C16H24N4O16Zn2·3(H2O)	F(000) = 1464
Mr = 713.18	Dx = 2.021 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 15.819 (4) Å	Cell parameters from 332 reflections
b = 10.4316 (10) Å	θ = 3.8–27.0°
c = 14.2229 (13) Å	µ = 2.15 mm^−1
β = 93.03 (3)°	T = 296 K
V = 2343.8 (6) Å^3	Plate, colourless
Z = 4	0.20 × 0.15 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.068
Radiation source: sealed x-ray tube	θmax = 27.0°, θmin = 3.8°
ω scan	h = −3→3
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −12→13
Tmin = 0.685, Tmax = 0.898	l = −17→17
4678 measured reflections	12 standard reflections every 84 reflections
429 independent reflections	intensity decay: none
332 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.032	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.081	w = 1/[σ^2(Fo^2) + (0.0472P)^2 + 6.8691P] where P = (Fo^2 + 2Fc^2)/3
S = 1.11	(Δ/σ)max = 0.001
429 reflections	Δρmax = 0.14 e Å^−3
196 parameters	Δρmin = −0.18 e Å^−3
130 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 1.82 (2) GPa (1820000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7344 (3)	0.50599 (9)	0.45303 (6)	0.0301 (19)
O4	0.683 (3)	0.8665 (8)	0.5511 (6)	0.037 (3)
O2	0.5420 (15)	0.7604 (5)	0.3999 (4)	0.034 (4)
O1	0.640 (2)	0.6081 (6)	0.4072 (4)	0.036 (3)
O14	0.7485 (18)	0.0441 (7)	0.4128 (5)	0.048 (3)
O11	0.7563 (19)	0.3787 (6)	0.3593 (4)	0.050 (3)
O13	0.870 (2)	0.1402 (6)	0.4581 (5)	0.042 (4)
O12	0.629 (3)	0.3409 (12)	0.2980 (8)	0.053 (6)
O3	0.5727 (19)	1.0083 (5)	0.5852 (5)	0.043 (4)
N13	0.892 (2)	0.2472 (7)	0.2906 (5)	0.032 (4)
H13A	0.9063	0.2545	0.2312	0.039*
H13B	0.9359	0.2187	0.3261	0.039*
H13C	0.8761	0.3234	0.3117	0.039*
O1W	0.593 (2)	0.9883 (10)	0.3171 (9)	0.066 (5)
H1WA	0.6523	0.9747	0.3405	0.099*
H1WB	0.5771	0.9419	0.3659	0.099*
N3	0.459 (2)	0.8194 (10)	0.5680 (6)	0.044 (5)
H3A	0.4546	0.8342	0.5063	0.053*
H3B	0.4444	0.8897	0.5987	0.053*
H3C	0.4245	0.7554	0.5819	0.053*
O2W	0.5000	0.5238 (12)	0.2500	0.054 (5)
C1	0.580 (3)	0.6788 (9)	0.4444 (6)	0.031 (3)
C4	0.605 (4)	0.8995 (11)	0.5730 (8)	0.023 (4)
C11	0.698 (4)	0.3174 (15)	0.3046 (10)	0.024 (4)
C14	0.810 (3)	0.1132 (9)	0.3981 (7)	0.027 (3)
C13	0.820 (3)	0.1544 (8)	0.2955 (6)	0.029 (3)
H13	0.8340	0.0779	0.2596	0.034*
C3	0.547 (2)	0.7844 (10)	0.5962 (8)	0.030 (4)
H3	0.5506	0.7709	0.6644	0.036*
C12	0.740 (3)	0.2093 (8)	0.2512 (6)	0.029 (3)
H12A	0.6988	0.1403	0.2426	0.034*
H12B	0.7515	0.2408	0.1891	0.034*
C2	0.570 (2)	0.6619 (7)	0.5493 (5)	0.028 (3)
H2A	0.5266	0.5983	0.5591	0.034*
H2B	0.6228	0.6302	0.5782	0.034*
H2W	0.547 (6)	0.483 (10)	0.257 (17)	0.16 (8)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.033 (6)	0.0294 (7)	0.0274 (6)	0.0010 (16)	−0.0029 (15)	−0.0006 (4)
O4	0.037 (6)	0.035 (3)	0.040 (4)	−0.003 (5)	0.002 (5)	−0.004 (3)
O2	0.032 (12)	0.033 (3)	0.035 (3)	0.002 (7)	−0.008 (6)	0.003 (3)
O1	0.036 (6)	0.038 (3)	0.034 (3)	0.001 (4)	0.001 (4)	0.000 (3)
O14	0.048 (6)	0.049 (3)	0.046 (3)	−0.002 (4)	0.003 (4)	0.011 (3)
O11	0.050 (6)	0.047 (3)	0.053 (3)	0.000 (4)	0.002 (4)	−0.019 (3)
O13	0.040 (12)	0.049 (4)	0.037 (3)	−0.003 (8)	0.000 (8)	0.003 (3)
O12	0.052 (12)	0.049 (6)	0.056 (6)	−0.001 (8)	0.001 (8)	−0.008 (4)
O3	0.043 (12)	0.032 (3)	0.055 (3)	0.002 (7)	0.005 (8)	0.000 (3)
N13	0.032 (12)	0.036 (4)	0.029 (4)	0.000 (8)	0.008 (7)	0.007 (3)
O1W	0.067 (12)	0.052 (4)	0.082 (6)	−0.002 (8)	0.029 (8)	−0.013 (4)
N3	0.045 (12)	0.043 (5)	0.045 (5)	0.004 (8)	0.003 (8)	−0.010 (4)
O2W	0.053 (12)	0.038 (5)	0.071 (6)	0.000	−0.005 (9)	0.000
C1	0.032 (6)	0.031 (4)	0.031 (4)	−0.002 (5)	0.001 (5)	0.000 (3)
C4	0.023 (7)	0.024 (4)	0.022 (4)	−0.001 (5)	0.001 (5)	−0.002 (3)
C11	0.024 (7)	0.025 (5)	0.023 (5)	0.001 (5)	0.002 (5)	0.002 (3)
C14	0.027 (6)	0.023 (4)	0.032 (4)	−0.001 (5)	0.003 (5)	−0.002 (3)
C13	0.029 (6)	0.031 (4)	0.027 (3)	0.001 (5)	0.002 (4)	−0.003 (3)
C3	0.030 (7)	0.031 (4)	0.029 (4)	0.000 (5)	0.002 (5)	−0.002 (3)
C12	0.029 (6)	0.030 (3)	0.027 (3)	0.000 (5)	0.001 (5)	−0.001 (3)
C2	0.028 (6)	0.026 (3)	0.030 (3)	0.000 (4)	−0.001 (5)	0.001 (3)

Geometric parameters (Å, º)

Zn1—O4^i	1.87 (4)	N3—H3A	0.8900
Zn1—O1	1.92 (4)	N3—H3B	0.8900
Zn1—O14^ii	1.983 (8)	N3—H3C	0.8900
Zn1—O11	1.926 (9)	N3—C3	1.47 (5)
Zn1—C14^ii	2.584 (19)	O2W—H2W	0.86 (6)
O4—C4	1.33 (8)	O2W—H2W^iii	0.86 (6)
O2—C1	1.20 (3)	C1—C2	1.518 (16)
O1—C1	1.34 (5)	C4—C3	1.56 (4)
O14—C14	1.24 (5)	C11—C12	1.53 (5)
O11—C11	1.34 (5)	C14—C13	1.536 (16)
O13—C14	1.27 (5)	C13—H13	0.9800
O12—C11	1.12 (10)	C13—C12	1.50 (6)
O3—C4	1.26 (3)	C3—H3	0.9800
N13—H13A	0.8900	C3—C2	1.497 (19)
N13—H13B	0.8900	C12—H12A	0.9700
N13—H13C	0.8900	C12—H12B	0.9700
N13—C13	1.50 (5)	C2—H2A	0.9700
O1W—H1WA	0.9959	C2—H2B	0.9700
O1W—H1WB	0.8901
O4^i—Zn1—O1	97.4 (14)	O11—C11—C12	110 (5)
O4^i—Zn1—O14^ii	99.0 (9)	O12—C11—O11	126 (2)
O4^i—Zn1—O11	108.4 (11)	O12—C11—C12	124 (4)
O4^i—Zn1—C14^ii	126.1 (9)	O14—C14—Zn1^ii	48.1 (8)
O1—Zn1—O14^ii	122.5 (9)	O14—C14—O13	125.4 (14)
O1—Zn1—O11	108.2 (8)	O14—C14—C13	116 (3)
O1—Zn1—C14^ii	107.8 (10)	O13—C14—Zn1^ii	77.4 (10)
O14^ii—Zn1—C14^ii	27.6 (13)	O13—C14—C13	118 (4)
O11—Zn1—O14^ii	117.7 (5)	C13—C14—Zn1^ii	163 (2)
O11—Zn1—C14^ii	107.6 (4)	N13—C13—C14	110 (3)
C4—O4—Zn1^i	118.8 (12)	N13—C13—H13	107.7
C1—O1—Zn1	136.9 (11)	N13—C13—C12	111.3 (17)
C14—O14—Zn1^ii	104.3 (17)	C14—C13—H13	107.7
C11—O11—Zn1	126 (3)	C12—C13—C14	112 (3)
H13A—N13—H13B	109.5	C12—C13—H13	107.7
H13A—N13—H13C	109.5	N3—C3—C4	108 (2)
H13B—N13—H13C	109.5	N3—C3—H3	108.3
C13—N13—H13A	109.5	N3—C3—C2	110 (2)
C13—N13—H13B	109.5	C4—C3—H3	108.3
C13—N13—H13C	109.5	C2—C3—C4	114 (3)
H1WA—O1W—H1WB	87.5	C2—C3—H3	108.3
H3A—N3—H3B	109.5	C11—C12—H12A	108.1
H3A—N3—H3C	109.5	C11—C12—H12B	108.1
H3B—N3—H3C	109.5	C13—C12—C11	117 (3)
C3—N3—H3A	109.5	C13—C12—H12A	108.1
C3—N3—H3B	109.5	C13—C12—H12B	108.1
C3—N3—H3C	109.5	H12A—C12—H12B	107.3
H2W—O2W—H2W^iii	120 (10)	C1—C2—H2A	109.2
O2—C1—O1	121.8 (16)	C1—C2—H2B	109.2
O2—C1—C2	122 (3)	C3—C2—C1	112.2 (10)
O1—C1—C2	116 (3)	C3—C2—H2A	109.2
O4—C4—C3	114.5 (19)	C3—C2—H2B	109.2
O3—C4—O4	131 (4)	H2A—C2—H2B	107.9
O3—C4—C3	115 (4)
Zn1—O1—C1—C2	−13 (5)	N3—C3—C4—O3	36 (2)
Zn1—O11—C11—C12	−170.9 (11)	C1—C2—C3—N3	71 (4)
O2—C1—C2—C3	−27 (5)	C1—C2—C3—C4	−50 (4)
O12—C11—C12—C13	−154 (3)	C11—C12—C13—N13	−71 (3)
N13—C13—C14—O13	−13 (3)	C11—C12—C13—C14	52 (3)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1; (iii) −x+1, y, −z+1/2.

(Zn-aspartate_sesquihydrate_2_15GPa)

Crystal data

C16H24N4O16Zn2·3(H2O)	F(000) = 1464
Mr = 713.18	Dx = 2.044 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 15.782 (4) Å	Cell parameters from 316 reflections
b = 10.3838 (9) Å	θ = 3.8–26.7°
c = 14.1615 (13) Å	µ = 2.18 mm^−1
β = 92.99 (3)°	T = 296 K
V = 2317.5 (6) Å^3	Plate, colourless
Z = 4	0.20 × 0.15 × 0.04 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.069
Radiation source: sealed x-ray tube	θmax = 26.7°, θmin = 3.8°
ω scan	h = −3→3
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −12→13
Tmin = 0.682, Tmax = 0.917	l = −17→17
4622 measured reflections	12 standard reflections every 84 reflections
427 independent reflections	intensity decay: none
316 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.034	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.070	w = 1/[σ^2(Fo^2) + 27.4439P] where P = (Fo^2 + 2Fc^2)/3
S = 1.10	(Δ/σ)max < 0.001
427 reflections	Δρmax = 0.17 e Å^−3
199 parameters	Δρmin = −0.16 e Å^−3
134 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 2.15 (2) GPa (2150000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7355 (4)	0.50599 (11)	0.45344 (7)	0.039 (6)
O4	0.683 (2)	0.8657 (8)	0.5513 (6)	0.040 (3)
O2	0.5414 (17)	0.7599 (6)	0.4006 (4)	0.033 (4)
O1	0.642 (3)	0.6066 (7)	0.4073 (5)	0.038 (3)
O14	0.745 (2)	0.0442 (8)	0.4122 (5)	0.049 (3)
O11	0.757 (2)	0.3785 (7)	0.3585 (5)	0.054 (3)
O13	0.868 (2)	0.1383 (7)	0.4579 (5)	0.040 (4)
O12	0.623 (2)	0.3410 (11)	0.2964 (8)	0.049 (6)
O3	0.571 (2)	1.0081 (6)	0.5866 (5)	0.041 (4)
N13	0.888 (2)	0.2458 (8)	0.2892 (5)	0.034 (4)
H13A	0.9008	0.2569	0.2292	0.040*
H13B	0.9359	0.2261	0.3282	0.037*
H13C	0.8731	0.3209	0.3135	0.040*
O1W	0.592 (2)	0.9889 (11)	0.3148 (7)	0.071 (9)
H1WA	0.640 (6)	0.982 (17)	0.343 (15)	0.106*
H1WB	0.560 (8)	0.936 (9)	0.341 (12)	0.106*
N3	0.459 (3)	0.8188 (11)	0.5693 (7)	0.040 (5)
H3A	0.4569	0.8514	0.5111	0.048*
H3B	0.4404	0.8772	0.6093	0.048*
H3C	0.4262	0.7490	0.5704	0.048*
O2W	0.5000	0.5236 (15)	0.2500	0.060 (6)
C1	0.580 (3)	0.6767 (9)	0.4444 (6)	0.029 (3)
C4	0.600 (2)	0.8992 (11)	0.5728 (8)	0.027 (4)
C11	0.703 (3)	0.3181 (16)	0.3042 (11)	0.027 (5)
C14	0.815 (3)	0.1144 (12)	0.3972 (8)	0.034 (4)
C13	0.819 (2)	0.1542 (9)	0.2942 (6)	0.026 (3)
H13	0.8338	0.0777	0.2581	0.031*
C3	0.546 (2)	0.7837 (11)	0.5973 (9)	0.036 (4)
H3	0.5510	0.7706	0.6659	0.043*
C12	0.739 (3)	0.2086 (9)	0.2490 (7)	0.030 (3)
H12A	0.6971	0.1405	0.2422	0.036*
H12B	0.7505	0.2390	0.1862	0.036*
C2	0.568 (2)	0.6613 (8)	0.5498 (5)	0.023 (3)
H2A	0.5231	0.5993	0.5586	0.028*
H2B	0.6198	0.6269	0.5799	0.028*
H2W	0.546 (8)	0.482 (14)	0.241 (12)	0.10 (9)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.058 (19)	0.0298 (7)	0.0269 (7)	−0.001 (2)	−0.0031 (17)	−0.0003 (5)
O4	0.040 (6)	0.034 (3)	0.045 (4)	−0.003 (4)	0.000 (4)	−0.001 (3)
O2	0.033 (11)	0.035 (3)	0.031 (3)	0.000 (7)	−0.004 (7)	0.002 (3)
O1	0.038 (6)	0.043 (3)	0.033 (3)	0.002 (4)	0.000 (4)	−0.001 (3)
O14	0.049 (6)	0.054 (4)	0.045 (3)	−0.001 (4)	0.003 (4)	0.006 (3)
O11	0.054 (6)	0.054 (4)	0.054 (4)	−0.001 (4)	0.004 (4)	−0.014 (3)
O13	0.039 (11)	0.050 (4)	0.032 (3)	−0.006 (8)	0.002 (8)	0.004 (3)
O12	0.049 (12)	0.047 (6)	0.051 (6)	0.004 (8)	0.002 (8)	−0.004 (4)
O3	0.042 (11)	0.035 (4)	0.047 (4)	0.003 (7)	0.010 (8)	0.001 (3)
N13	0.033 (11)	0.034 (4)	0.034 (4)	0.001 (8)	0.009 (8)	0.003 (4)
O1W	0.07 (3)	0.048 (5)	0.096 (7)	−0.024 (12)	0.056 (13)	−0.018 (5)
N3	0.040 (12)	0.040 (5)	0.038 (5)	0.004 (8)	0.003 (8)	−0.008 (4)
O2W	0.058 (12)	0.048 (6)	0.072 (7)	0.000	0.001 (8)	0.000
C1	0.029 (6)	0.030 (4)	0.029 (4)	−0.002 (5)	0.002 (5)	0.001 (3)
C4	0.027 (7)	0.026 (5)	0.027 (4)	−0.001 (5)	0.003 (5)	0.000 (3)
C11	0.027 (7)	0.027 (5)	0.027 (5)	0.001 (5)	0.002 (5)	0.002 (3)
C14	0.034 (6)	0.034 (4)	0.035 (4)	0.001 (5)	0.002 (4)	−0.001 (4)
C13	0.025 (6)	0.028 (4)	0.024 (4)	0.000 (4)	0.002 (4)	0.002 (3)
C3	0.036 (7)	0.038 (5)	0.033 (5)	−0.001 (5)	0.001 (5)	−0.003 (3)
C12	0.030 (6)	0.032 (4)	0.029 (4)	0.000 (5)	0.001 (4)	−0.003 (3)
C2	0.023 (6)	0.022 (3)	0.024 (4)	0.000 (4)	0.001 (4)	−0.001 (3)

Geometric parameters (Å, º)

Zn1—O4^i	1.85 (3)	O12—C11	1.28 (6)
Zn1—O1	1.90 (4)	O3—C4	1.24 (2)
Zn1—O14^ii	1.981 (10)	N13—C13	1.456 (13)
Zn1—O11	1.930 (11)	N3—C3	1.46 (5)
O4—C4	1.400 (14)	C1—C2	1.522 (16)
O2—C1	1.20 (3)	C4—C3	1.52 (4)
O1—C1	1.35 (5)	C11—C12	1.51 (4)
O14—C14	1.34 (6)	C14—C13	1.521 (17)
O11—C11	1.29 (4)	C13—C12	1.49 (6)
O13—C14	1.20 (5)	C3—C2	1.49 (2)
O4^i—Zn1—O1	96.9 (11)	O3—C4—C3	118 (3)
O4^i—Zn1—O14^ii	98.5 (9)	O11—C11—C12	115 (4)
O4^i—Zn1—O11	108.7 (12)	O12—C11—O11	126 (3)
O1—Zn1—O14^ii	123.8 (11)	O12—C11—C12	120 (3)
O1—Zn1—O11	107.5 (9)	O14—C14—C13	112 (3)
O11—Zn1—O14^ii	117.7 (6)	O13—C14—O14	123.5 (18)
C4—O4—Zn1^i	118.9 (12)	O13—C14—C13	124 (4)
C1—O1—Zn1	136.9 (11)	N13—C13—C14	107 (2)
C14—O14—Zn1^ii	101.8 (19)	N13—C13—C12	110.6 (17)
C11—O11—Zn1	128 (3)	C12—C13—C14	116 (3)
O2—C1—O1	122.6 (16)	N3—C3—C4	106 (2)
O2—C1—C2	120 (3)	N3—C3—C2	109 (2)
O1—C1—C2	117 (2)	C2—C3—C4	115 (3)
O4—C4—C3	113 (2)	C13—C12—C11	113 (2)
O3—C4—O4	128 (2)	C3—C2—C1	113.2 (10)
Zn1—O1—C1—C2	−12 (5)	N3—C3—C4—O3	38.7 (19)
Zn1—O11—C11—C12	−170.3 (11)	C1—C2—C3—N3	73 (4)
O2—C1—C2—C3	−29 (5)	C1—C2—C3—C4	−46 (5)
O12—C11—C12—C13	−154 (3)	C11—C12—C13—N13	−70 (3)
N13—C13—C14—O13	−11 (3)	C11—C12—C13—C14	53 (3)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1.

(Zn-aspartate_sesquihydrate_2_49GPa)

Crystal data

C16H24N4O16Zn2·3(H2O)	F(000) = 1464
Mr = 713.18	Dx = 2.063 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 15.731 (3) Å	Cell parameters from 320 reflections
b = 10.3513 (6) Å	θ = 3.8–26.7°
c = 14.1190 (9) Å	µ = 2.20 mm^−1
β = 92.92 (2)°	T = 296 K
V = 2296.1 (4) Å^3	Plate, colourless
Z = 4	0.20 × 0.15 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.069
Radiation source: sealed x-ray tube	θmax = 26.7°, θmin = 3.8°
ω scan	h = −3→3
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −12→13
Tmin = 0.680, Tmax = 0.896	l = −17→17
4599 measured reflections	12 standard reflections every 84 reflections
424 independent reflections	intensity decay: none
320 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.029	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.067	w = 1/[σ^2(Fo^2) + (0.0339P)^2 + 6.1011P] where P = (Fo^2 + 2Fc^2)/3
S = 1.11	(Δ/σ)max < 0.001
424 reflections	Δρmax = 0.14 e Å^−3
199 parameters	Δρmin = −0.13 e Å^−3
129 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 2.49 (2) GPa (2490000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7360 (3)	0.50630 (9)	0.45372 (6)	0.040 (6)
O4	0.685 (2)	0.8655 (8)	0.5507 (6)	0.040 (3)
O2	0.5401 (14)	0.7607 (5)	0.4008 (3)	0.033 (4)
O1	0.642 (2)	0.6070 (6)	0.4075 (4)	0.036 (3)
O14	0.7471 (19)	0.0438 (8)	0.4116 (5)	0.053 (3)
O11	0.7581 (18)	0.3799 (6)	0.3580 (4)	0.052 (3)
O13	0.8679 (19)	0.1397 (6)	0.4576 (4)	0.041 (4)
O12	0.6234 (19)	0.3416 (10)	0.2969 (7)	0.053 (6)
O3	0.5710 (18)	1.0083 (5)	0.5867 (4)	0.041 (4)
N13	0.891 (2)	0.2463 (6)	0.2890 (5)	0.035 (4)
H13A	0.9036	0.2570	0.2288	0.042*
H13B	0.9359	0.2261	0.3282	0.037*
H13C	0.8764	0.3221	0.3133	0.042*
O1W	0.588 (2)	0.9893 (8)	0.3129 (6)	0.072 (5)
H1WA	0.636 (6)	0.978 (14)	0.347 (13)	0.098*
H1WB	0.555 (6)	0.936 (8)	0.338 (10)	0.098*
N3	0.461 (3)	0.8194 (9)	0.5691 (6)	0.034 (5)
H3A	0.4608	0.8449	0.5102	0.044*
H3B	0.4427	0.8787	0.6087	0.041*
H3C	0.4344	0.7541	0.5766	0.044*
O2W	0.5000	0.5261 (11)	0.2500	0.055 (5)
C1	0.583 (3)	0.6778 (9)	0.4455 (6)	0.027 (3)
C4	0.598 (3)	0.8988 (11)	0.5724 (8)	0.028 (4)
C11	0.702 (2)	0.3200 (14)	0.3029 (10)	0.025 (4)
C14	0.811 (3)	0.1132 (9)	0.3974 (7)	0.029 (3)
C13	0.818 (3)	0.1541 (8)	0.2939 (6)	0.027 (3)
H13	0.8320	0.0769	0.2578	0.032*
C3	0.542 (3)	0.7827 (10)	0.5982 (8)	0.035 (4)
H3	0.5445	0.7708	0.6671	0.042*
C12	0.736 (3)	0.2091 (8)	0.2491 (6)	0.031 (3)
H12A	0.7466	0.2374	0.1852	0.037*
H12B	0.6937	0.1411	0.2444	0.037*
C2	0.569 (2)	0.6591 (7)	0.5511 (5)	0.029 (3)
H2A	0.5255	0.5936	0.5585	0.034*
H2B	0.6212	0.6285	0.5825	0.034*
H2W	0.542 (6)	0.475 (8)	0.238 (8)	0.09 (6)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.065 (17)	0.0282 (6)	0.0267 (6)	−0.0024 (17)	−0.0024 (15)	−0.0006 (4)
O4	0.040 (6)	0.034 (3)	0.045 (4)	−0.006 (5)	−0.001 (5)	−0.004 (3)
O2	0.031 (12)	0.037 (3)	0.030 (3)	0.002 (7)	−0.013 (6)	0.003 (2)
O1	0.036 (6)	0.041 (3)	0.029 (3)	0.001 (5)	−0.003 (4)	0.002 (2)
O14	0.053 (6)	0.058 (3)	0.047 (3)	−0.001 (5)	0.003 (4)	0.011 (3)
O11	0.052 (6)	0.050 (3)	0.055 (3)	0.000 (4)	0.003 (5)	−0.016 (3)
O13	0.039 (12)	0.045 (3)	0.038 (3)	−0.003 (8)	−0.001 (8)	0.000 (3)
O12	0.053 (12)	0.051 (6)	0.056 (5)	−0.001 (9)	0.007 (9)	−0.001 (4)
O3	0.040 (12)	0.034 (3)	0.048 (3)	0.009 (7)	0.008 (8)	−0.003 (3)
N13	0.035 (12)	0.036 (4)	0.034 (4)	−0.001 (8)	0.008 (8)	0.007 (3)
O1W	0.074 (12)	0.051 (4)	0.092 (5)	−0.008 (7)	0.028 (8)	−0.017 (4)
N3	0.034 (12)	0.035 (4)	0.032 (4)	0.006 (8)	0.002 (8)	−0.006 (4)
O2W	0.053 (12)	0.036 (5)	0.076 (6)	0.000	−0.008 (8)	0.000
C1	0.027 (6)	0.029 (4)	0.026 (4)	−0.002 (5)	0.003 (5)	−0.001 (3)
C4	0.028 (7)	0.026 (4)	0.031 (4)	−0.002 (5)	0.004 (5)	−0.001 (3)
C11	0.024 (7)	0.024 (5)	0.025 (5)	0.001 (5)	0.001 (5)	−0.002 (3)
C14	0.029 (6)	0.025 (4)	0.033 (4)	0.001 (5)	0.002 (5)	−0.002 (3)
C13	0.027 (6)	0.029 (3)	0.025 (3)	0.000 (5)	0.002 (5)	−0.001 (3)
C3	0.035 (7)	0.036 (5)	0.034 (4)	−0.001 (5)	0.002 (5)	−0.001 (3)
C12	0.031 (6)	0.032 (3)	0.030 (4)	−0.001 (5)	0.003 (5)	0.001 (3)
C2	0.028 (6)	0.028 (3)	0.030 (3)	0.000 (5)	0.000 (5)	0.000 (3)

Geometric parameters (Å, º)

Zn1—O4^i	1.83 (3)	N3—H3A	0.8700
Zn1—O1	1.90 (3)	N3—H3B	0.8900
Zn1—O14^ii	1.977 (8)	N3—H3C	0.8000
Zn1—O11	1.923 (9)	N3—C3	1.38 (7)
Zn1—C14^ii	2.574 (18)	O2W—H2W	0.86 (6)
O4—C4	1.45 (6)	O2W—H2W^iii	0.86 (6)
O2—C1	1.24 (3)	C1—C2	1.530 (17)
O1—C1	1.32 (5)	C4—C3	1.54 (5)
O14—C14	1.26 (5)	C11—C12	1.49 (3)
O11—C11	1.31 (3)	C14—C13	1.532 (14)
O13—C14	1.25 (4)	C13—H13	0.9800
O12—C11	1.25 (3)	C13—C12	1.53 (5)
O3—C4	1.23 (2)	C3—H3	0.9800
N13—H13A	0.8900	C3—C2	1.51 (2)
N13—H13B	0.8900	C12—H12A	0.9700
N13—H13C	0.8900	C12—H12B	0.9700
N13—C13	1.48 (4)	C2—H2A	0.9700
O1W—H1WA	0.87 (7)	C2—H2B	0.9700
O1W—H1WB	0.83 (6)
O4^i—Zn1—O1	96.4 (11)	O11—C11—C12	115 (3)
O4^i—Zn1—O14^ii	99.1 (8)	O12—C11—O11	126 (2)
O4^i—Zn1—O11	108.7 (10)	O12—C11—C12	118 (2)
O4^i—Zn1—C14^ii	126.6 (8)	O14—C14—Zn1^ii	48.4 (7)
O1—Zn1—O14^ii	122.9 (9)	O14—C14—C13	115 (3)
O1—Zn1—O11	107.3 (8)	O13—C14—Zn1^ii	77.0 (10)
O1—Zn1—C14^ii	107.4 (9)	O13—C14—O14	125.4 (14)
O14^ii—Zn1—C14^ii	28.4 (12)	O13—C14—C13	120 (3)
O11—Zn1—O14^ii	118.5 (4)	C13—C14—Zn1^ii	162 (2)
O11—Zn1—C14^ii	108.4 (4)	N13—C13—C14	109 (2)
C4—O4—Zn1^i	119.0 (11)	N13—C13—H13	107.5
C1—O1—Zn1	135.9 (11)	N13—C13—C12	112.2 (15)
C14—O14—Zn1^ii	103.2 (16)	C14—C13—H13	107.5
C11—O11—Zn1	127 (2)	C12—C13—C14	113 (3)
H13A—N13—H13B	114.0	C12—C13—H13	107.5
H13A—N13—H13C	109.5	N3—C3—C4	104 (2)
H13B—N13—H13C	100.0	N3—C3—H3	109.4
C13—N13—H13A	109.5	N3—C3—C2	112 (2)
C13—N13—H13B	114.0	C4—C3—H3	109.4
C13—N13—H13C	109.5	C2—C3—C4	113 (3)
H1WA—O1W—H1WB	103 (10)	C2—C3—H3	109.4
H3A—N3—H3B	114.0	C11—C12—C13	113.0 (18)
H3A—N3—H3C	114.0	C11—C12—H12A	109.0
H3B—N3—H3C	108.0	C11—C12—H12B	109.0
C3—N3—H3A	109.5	C13—C12—H12A	109.0
C3—N3—H3B	109.5	C13—C12—H12B	109.0
C3—N3—H3C	102.0	H12A—C12—H12B	107.8
H2W—O2W—H2W^iii	106 (10)	C1—C2—H2A	109.2
O2—C1—O1	123.3 (13)	C1—C2—H2B	109.2
O2—C1—C2	119 (3)	C3—C2—C1	112.2 (10)
O1—C1—C2	118 (2)	C3—C2—H2A	109.2
O4—C4—C3	114 (2)	C3—C2—H2B	109.2
O3—C4—O4	126 (3)	H2A—C2—H2B	107.9
O3—C4—C3	118 (4)
Zn1—O1—C1—C2	−16 (5)	N3—C3—C4—O3	41 (2)
Zn1—O11—C11—C12	−168.6 (9)	C1—C2—C3—N3	70 (4)
O2—C1—C2—C3	−31 (5)	C1—C2—C3—C4	−47 (4)
O12—C11—C12—C13	−153 (2)	C11—C12—C13—N13	−67 (2)
N13—C13—C14—O13	−12 (3)	C11—C12—C13—C14	56 (2)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1; (iii) −x+1, y, −z+1/2.

(Zn-aspartate_sesquihydrate_2_91GPa)

Crystal data

C16H24N4O16Zn2·3(H2O)	F(000) = 1464
Mr = 713.18	Dx = 2.086 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 15.680 (3) Å	Cell parameters from 312 reflections
b = 10.3060 (8) Å	θ = 3.8–26.8°
c = 14.0720 (12) Å	µ = 2.22 mm^−1
β = 92.80 (3)°	T = 296 K
V = 2271.3 (6) Å^3	Plate, colourless
Z = 4	0.20 × 0.15 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.071
Radiation source: sealed x-ray tube	θmax = 26.8°, θmin = 3.8°
ω scan	h = −3→3
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −12→12
Tmin = 0.677, Tmax = 0.895	l = −17→17
4527 measured reflections	12 standard reflections every 84 reflections
413 independent reflections	intensity decay: none
312 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.032	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.062	w = 1/[σ^2(Fo^2) + 21.7186P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max < 0.001
413 reflections	Δρmax = 0.13 e Å^−3
199 parameters	Δρmin = −0.12 e Å^−3
130 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 2.91 (2) GPa (2910000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7366 (3)	0.50612 (10)	0.45405 (7)	0.048 (6)
O4	0.679 (2)	0.8643 (8)	0.5506 (6)	0.038 (3)
O2	0.5389 (16)	0.7599 (6)	0.4017 (4)	0.034 (4)
O1	0.640 (2)	0.6060 (7)	0.4081 (5)	0.035 (3)
O14	0.742 (2)	0.0430 (8)	0.4107 (5)	0.054 (3)
O11	0.757 (2)	0.3808 (7)	0.3574 (5)	0.054 (3)
O13	0.867 (2)	0.1395 (7)	0.4578 (5)	0.040 (4)
O12	0.622 (2)	0.3419 (11)	0.2958 (8)	0.051 (6)
O3	0.5720 (19)	1.0086 (6)	0.5868 (5)	0.040 (4)
N13	0.892 (2)	0.2459 (7)	0.2884 (5)	0.035 (4)
H13A	0.9061	0.2544	0.2283	0.042*
H13B	0.9357	0.2148	0.3235	0.042*
H13C	0.8768	0.3230	0.3109	0.042*
O1W	0.587 (2)	0.9892 (10)	0.3112 (6)	0.071 (5)
H1WA	0.634 (7)	0.980 (16)	0.347 (14)	0.106*
H1WB	0.554 (8)	0.938 (8)	0.342 (12)	0.106*
N3	0.457 (3)	0.8189 (11)	0.5683 (7)	0.037 (5)
H3A	0.4570	0.8500	0.5092	0.044*
H3B	0.4384	0.8796	0.6071	0.044*
H3C	0.4233	0.7497	0.5696	0.044*
O2W	0.5000	0.5250 (11)	0.2500	0.054 (5)
C1	0.581 (4)	0.6760 (10)	0.4459 (6)	0.029 (3)
C4	0.600 (2)	0.8984 (13)	0.5727 (8)	0.028 (4)
C11	0.701 (3)	0.3204 (16)	0.3037 (11)	0.028 (5)
C14	0.815 (3)	0.1122 (11)	0.3974 (8)	0.030 (3)
C13	0.817 (3)	0.1535 (9)	0.2926 (6)	0.028 (3)
H13	0.8310	0.0762	0.2560	0.034*
C3	0.541 (4)	0.7829 (11)	0.5982 (9)	0.032 (4)
H3	0.5443	0.7710	0.6674	0.038*
C12	0.739 (3)	0.2089 (10)	0.2475 (7)	0.035 (3)
H12A	0.6967	0.1408	0.2392	0.042*
H12B	0.7518	0.2405	0.1848	0.042*
C2	0.566 (2)	0.6581 (8)	0.5517 (5)	0.029 (3)
H2A	0.5219	0.5941	0.5593	0.035*
H2B	0.6185	0.6255	0.5833	0.035*
H2W	0.545 (9)	0.477 (14)	0.238 (10)	0.10 (10)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.086 (18)	0.0289 (7)	0.0276 (6)	0.001 (2)	−0.0031 (16)	−0.0001 (5)
O4	0.038 (6)	0.033 (4)	0.043 (4)	−0.005 (5)	0.000 (5)	−0.001 (3)
O2	0.034 (12)	0.038 (3)	0.030 (3)	−0.001 (7)	−0.008 (7)	0.002 (3)
O1	0.036 (6)	0.040 (3)	0.030 (3)	0.000 (5)	−0.002 (4)	0.003 (3)
O14	0.054 (6)	0.058 (4)	0.050 (3)	−0.003 (5)	0.002 (5)	0.011 (3)
O11	0.054 (6)	0.052 (3)	0.056 (4)	−0.002 (4)	0.003 (5)	−0.016 (3)
O13	0.039 (12)	0.049 (4)	0.032 (3)	−0.003 (8)	0.001 (8)	0.003 (3)
O12	0.051 (12)	0.048 (6)	0.054 (6)	−0.001 (9)	0.001 (9)	−0.001 (4)
O3	0.041 (12)	0.034 (4)	0.045 (4)	0.001 (8)	0.002 (8)	−0.001 (3)
N13	0.036 (12)	0.033 (4)	0.037 (4)	−0.002 (8)	0.010 (8)	0.001 (4)
O1W	0.071 (12)	0.053 (4)	0.089 (6)	−0.005 (8)	0.021 (8)	−0.021 (4)
N3	0.037 (12)	0.037 (5)	0.037 (5)	0.002 (9)	0.001 (8)	−0.005 (4)
O2W	0.053 (12)	0.036 (5)	0.072 (6)	0.000	−0.009 (8)	0.000
C1	0.029 (6)	0.030 (4)	0.029 (4)	−0.002 (5)	0.001 (5)	0.001 (3)
C4	0.028 (7)	0.028 (5)	0.029 (4)	0.000 (5)	0.003 (5)	−0.001 (4)
C11	0.027 (7)	0.028 (5)	0.027 (5)	0.001 (5)	0.001 (5)	−0.002 (3)
C14	0.030 (7)	0.028 (4)	0.033 (4)	0.000 (5)	0.001 (5)	−0.002 (3)
C13	0.029 (6)	0.029 (4)	0.028 (4)	−0.002 (5)	0.001 (5)	0.001 (3)
C3	0.032 (7)	0.033 (5)	0.031 (5)	−0.001 (5)	0.002 (5)	−0.001 (3)
C12	0.035 (6)	0.034 (4)	0.035 (4)	−0.001 (5)	0.001 (5)	0.003 (3)
C2	0.029 (6)	0.027 (3)	0.032 (4)	−0.001 (5)	0.002 (5)	−0.001 (3)

Geometric parameters (Å, º)

Zn1—O4^i	1.88 (3)	O12—C11	1.26 (6)
Zn1—O1	1.91 (3)	O3—C4	1.24 (3)
Zn1—O14^ii	1.983 (10)	N13—C13	1.51 (5)
Zn1—O11	1.914 (11)	N3—C3	1.42 (8)
Zn1—C14^ii	2.583 (18)	C1—C2	1.53 (2)
O4—C4	1.34 (3)	C4—C3	1.55 (5)
O2—C1	1.24 (4)	C11—C12	1.53 (4)
O1—C1	1.31 (6)	C14—C13	1.537 (15)
O14—C14	1.37 (5)	C13—C12	1.46 (6)
O11—C11	1.30 (4)	C3—C2	1.50 (2)
O13—C14	1.18 (4)
O4^i—Zn1—O1	98.7 (11)	O3—C4—C3	117 (4)
O4^i—Zn1—O14^ii	97.3 (10)	O11—C11—C12	113 (4)
O4^i—Zn1—O11	108.0 (11)	O12—C11—O11	128 (3)
O4^i—Zn1—C14^ii	127.6 (8)	O12—C11—C12	120 (3)
O1—Zn1—O14^ii	123.8 (11)	O14—C14—Zn1^ii	49.3 (8)
O1—Zn1—O11	106.3 (9)	O14—C14—C13	109 (3)
O1—Zn1—C14^ii	104.8 (10)	O13—C14—Zn1^ii	76.2 (12)
O14^ii—Zn1—C14^ii	31.5 (14)	O13—C14—O14	125.2 (17)
O11—Zn1—O14^ii	118.9 (6)	O13—C14—C13	125 (3)
O11—Zn1—C14^ii	109.1 (5)	C13—C14—Zn1^ii	158 (3)
C4—O4—Zn1^i	118.8 (12)	N13—C13—C14	105 (2)
C1—O1—Zn1	136.4 (13)	C12—C13—N13	111.6 (18)
C14—O14—Zn1^ii	99.2 (19)	C12—C13—C14	118 (3)
C11—O11—Zn1	127 (3)	N3—C3—C4	106 (2)
O2—C1—O1	123.5 (17)	N3—C3—C2	111 (3)
O2—C1—C2	118 (3)	C2—C3—C4	113 (4)
O1—C1—C2	118 (3)	C13—C12—C11	114 (2)
O4—C4—C3	114 (2)	C3—C2—C1	112.0 (12)
O3—C4—O4	128 (3)
Zn1—O1—C1—C2	−17 (6)	N3—C3—C4—O3	41 (2)
Zn1—O11—C11—C12	−169.2 (11)	C1—C2—C3—N3	71 (4)
O2—C1—C2—C3	−31 (6)	C1—C2—C3—C4	−48 (5)
O12—C11—C12—C13	−152 (3)	C11—C12—C13—N13	−71 (3)
N13—C13—C14—O13	−6 (4)	C11—C12—C13—C14	51 (3)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1.

(Zn-aspartate_sesquihydrate_3_54GPa)

Crystal data

C16H24N4O16Zn2·3(H2O)	F(000) = 1464
Mr = 713.18	Dx = 2.124 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 15.612 (4) Å	Cell parameters from 305 reflections
b = 10.2330 (9) Å	θ = 3.7–27.0°
c = 13.9799 (14) Å	µ = 2.26 mm^−1
β = 92.78 (3)°	T = 296 K
V = 2230.7 (7) Å^3	Plate, colourless
Z = 4	0.20 × 0.15 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.073
Radiation source: sealed x-ray tube	θmax = 27.0°, θmin = 3.7°
ω scan	h = −3→3
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −12→12
Tmin = 0.672, Tmax = 0.893	l = −17→17
4443 measured reflections	12 standard reflections every 84 reflections
413 independent reflections	intensity decay: none
305 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.033	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.057	w = 1/[σ^2(Fo^2) + 16.5695P] where P = (Fo^2 + 2Fc^2)/3
S = 1.14	(Δ/σ)max < 0.001
413 reflections	Δρmax = 0.12 e Å^−3
199 parameters	Δρmin = −0.18 e Å^−3
129 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 3.54 (2) GPa (3540000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7373 (3)	0.50605 (11)	0.45450 (7)	0.042 (6)
O4	0.679 (2)	0.8628 (8)	0.5499 (6)	0.036 (3)
O2	0.5378 (16)	0.7596 (6)	0.4021 (4)	0.030 (4)
O1	0.638 (3)	0.6046 (7)	0.4088 (4)	0.035 (3)
O14	0.741 (2)	0.0421 (8)	0.4093 (5)	0.053 (3)
O11	0.758 (2)	0.3814 (6)	0.3559 (5)	0.049 (3)
O13	0.866 (2)	0.1387 (7)	0.4579 (5)	0.037 (4)
O12	0.621 (2)	0.3439 (11)	0.2953 (8)	0.053 (6)
O3	0.5719 (18)	1.0088 (6)	0.5874 (4)	0.039 (4)
N13	0.891 (2)	0.2459 (7)	0.2872 (5)	0.032 (4)
H13A	0.9043	0.2556	0.2264	0.039*
H13B	0.9359	0.2130	0.3208	0.039*
H13C	0.8774	0.3232	0.3113	0.039*
O1W	0.583 (2)	0.9898 (10)	0.3089 (5)	0.066 (5)
H1WA	0.632 (7)	0.977 (15)	0.343 (15)	0.100*
H1WB	0.551 (8)	0.939 (8)	0.344 (12)	0.100*
N3	0.453 (3)	0.8198 (11)	0.5684 (6)	0.035 (5)
H3A	0.4608	0.8449	0.5102	0.044*
H3B	0.4318	0.8721	0.6123	0.042*
H3C	0.4200	0.7491	0.5615	0.042*
O2W	0.5000	0.5261 (12)	0.2500	0.051 (6)
C1	0.577 (4)	0.6765 (10)	0.4464 (6)	0.029 (3)
C4	0.603 (3)	0.8971 (13)	0.5727 (9)	0.027 (4)
C11	0.696 (2)	0.3207 (15)	0.3014 (11)	0.023 (4)
C14	0.809 (4)	0.1126 (11)	0.3969 (8)	0.030 (4)
C12	0.736 (3)	0.2089 (10)	0.2469 (7)	0.034 (4)
H12A	0.6943	0.1395	0.2386	0.041*
H12B	0.7492	0.2400	0.1836	0.041*
C13	0.815 (3)	0.1533 (8)	0.2925 (6)	0.024 (3)
H13	0.8290	0.0747	0.2563	0.029*
C3	0.537 (3)	0.7818 (10)	0.5982 (8)	0.026 (4)
H3	0.5398	0.7697	0.6678	0.031*
C2	0.561 (2)	0.6565 (8)	0.5528 (5)	0.029 (3)
H2A	0.5151	0.5936	0.5590	0.034*
H2B	0.6123	0.6215	0.5854	0.034*
H2W	0.547 (8)	0.480 (12)	0.235 (9)	0.10 (8)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.070 (19)	0.0278 (7)	0.0267 (6)	0.003 (2)	−0.0055 (16)	−0.0008 (5)
O4	0.036 (6)	0.031 (4)	0.039 (4)	−0.004 (5)	−0.001 (5)	−0.003 (3)
O2	0.028 (12)	0.033 (3)	0.029 (3)	−0.001 (7)	−0.005 (7)	0.001 (3)
O1	0.034 (6)	0.041 (3)	0.028 (3)	−0.002 (5)	−0.003 (4)	0.003 (3)
O14	0.053 (6)	0.059 (4)	0.048 (3)	−0.002 (5)	0.003 (5)	0.011 (3)
O11	0.049 (6)	0.044 (3)	0.054 (3)	−0.002 (4)	0.002 (5)	−0.013 (3)
O13	0.037 (12)	0.044 (4)	0.032 (3)	−0.004 (8)	0.004 (8)	0.002 (3)
O12	0.053 (12)	0.049 (6)	0.057 (6)	−0.001 (9)	0.005 (9)	0.000 (4)
O3	0.038 (12)	0.034 (4)	0.044 (3)	−0.003 (8)	0.003 (8)	−0.004 (3)
N13	0.033 (12)	0.029 (4)	0.035 (4)	−0.001 (8)	0.004 (8)	0.005 (3)
O1W	0.068 (12)	0.049 (4)	0.085 (5)	−0.005 (8)	0.028 (8)	−0.016 (4)
N3	0.036 (12)	0.037 (5)	0.033 (5)	0.000 (9)	0.008 (8)	−0.004 (4)
O2W	0.050 (12)	0.037 (6)	0.066 (6)	0.000	−0.009 (9)	0.000
C1	0.029 (7)	0.029 (4)	0.029 (4)	−0.002 (5)	0.003 (5)	−0.002 (3)
C4	0.027 (7)	0.026 (5)	0.028 (4)	0.000 (5)	0.004 (5)	−0.002 (4)
C11	0.022 (7)	0.024 (5)	0.022 (5)	0.001 (5)	0.001 (5)	−0.002 (3)
C14	0.031 (7)	0.027 (4)	0.034 (4)	0.001 (5)	0.000 (5)	−0.001 (4)
C12	0.034 (7)	0.037 (4)	0.032 (4)	0.000 (5)	0.001 (5)	0.002 (3)
C13	0.024 (6)	0.023 (4)	0.025 (3)	0.001 (5)	0.002 (5)	−0.003 (3)
C3	0.026 (7)	0.028 (4)	0.023 (4)	0.000 (5)	0.000 (5)	0.000 (3)
C2	0.028 (6)	0.028 (3)	0.028 (4)	0.000 (5)	−0.002 (5)	−0.004 (3)

Geometric parameters (Å, º)

Zn1—O4^i	1.88 (3)	O12—C11	1.20 (4)
Zn1—O1	1.93 (4)	O3—C4	1.26 (3)
Zn1—O14^ii	1.983 (10)	N13—C13	1.51 (5)
Zn1—O11	1.920 (11)	N3—C3	1.44 (8)
Zn1—C14^ii	2.54 (2)	C1—C2	1.53 (2)
O4—C4	1.30 (4)	C4—C3	1.60 (6)
O2—C1	1.20 (3)	C11—C12	1.53 (4)
O1—C1	1.33 (6)	C14—C13	1.526 (16)
O14—C14	1.31 (6)	C12—C13	1.48 (6)
O11—C11	1.36 (4)	C3—C2	1.49 (2)
O13—C14	1.24 (5)
O4^i—Zn1—O1	99.3 (11)	O3—C4—C3	112 (4)
O4^i—Zn1—O14^ii	96.6 (9)	O11—C11—C12	109 (4)
O4^i—Zn1—O11	107.9 (11)	O12—C11—O11	129 (2)
O4^i—Zn1—C14^ii	126.2 (10)	O12—C11—C12	123 (3)
O1—Zn1—O14^ii	123.4 (10)	O14—C14—Zn1^ii	50.6 (8)
O1—Zn1—C14^ii	105.5 (11)	O14—C14—C13	112 (3)
O14^ii—Zn1—C14^ii	30.6 (15)	O13—C14—Zn1^ii	76.4 (11)
O11—Zn1—O1	105.9 (9)	O13—C14—O14	126.9 (17)
O11—Zn1—O14^ii	119.9 (6)	O13—C14—C13	121 (4)
O11—Zn1—C14^ii	109.7 (4)	C13—C14—Zn1^ii	162 (3)
C4—O4—Zn1^i	117.6 (13)	C13—C12—C11	115.3 (19)
C1—O1—Zn1	137.4 (14)	N13—C13—C14	108 (3)
C14—O14—Zn1^ii	98.8 (18)	C12—C13—N13	112.0 (17)
C11—O11—Zn1	124 (3)	C12—C13—C14	115 (4)
O2—C1—O1	122.8 (18)	N3—C3—C4	109.0 (19)
O2—C1—C2	120 (3)	N3—C3—C2	110 (3)
O1—C1—C2	117 (3)	C2—C3—C4	112 (3)
O4—C4—C3	117 (2)	C3—C2—C1	110.6 (11)
O3—C4—O4	130 (3)
Zn1—O1—C1—C2	−20 (6)	N3—C3—C4—O3	39.1 (18)
Zn1—O11—C11—C12	−168.0 (10)	C1—C2—C3—N3	73 (4)
O2—C1—C2—C3	−32 (5)	C1—C2—C3—C4	−48 (4)
O12—C11—C12—C13	−152 (3)	C11—C12—C13—N13	−71 (3)
N13—C13—C14—O13	−10 (4)	C11—C12—C13—C14	53 (3)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1.

(Zn-aspartate_sesquihydrate_3_92GPa)

Crystal data

C16H24N4O16Zn2·3(H2O)	F(000) = 1464
Mr = 713.18	Dx = 2.135 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 15.550 (3) Å	Cell parameters from 292 reflections
b = 10.2262 (7) Å	θ = 3.7–27.1°
c = 13.9663 (11) Å	µ = 2.28 mm^−1
β = 92.62 (3)°	T = 296 K
V = 2218.6 (4) Å^3	Plate, colourless
Z = 4	0.20 × 0.15 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.077
Radiation source: sealed x-ray tube	θmax = 27.1°, θmin = 3.7°
ω scan	h = −3→3
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −12→12
Tmin = 0.671, Tmax = 0.892	l = −17→17
4400 measured reflections	12 standard reflections every 84 reflections
407 independent reflections	intensity decay: none
292 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.033	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.074	w = 1/[σ^2(Fo^2) + (0.0239P)^2 + 19.0079P] where P = (Fo^2 + 2Fc^2)/3
S = 1.10	(Δ/σ)max < 0.001
407 reflections	Δρmax = 0.15 e Å^−3
196 parameters	Δρmin = −0.18 e Å^−3
125 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 3.92 (2) GPa (3920000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7371 (5)	0.50611 (13)	0.45476 (9)	0.039 (8)
O4	0.683 (3)	0.8608 (11)	0.5494 (7)	0.039 (4)
O2	0.538 (2)	0.7597 (7)	0.4025 (5)	0.031 (5)
O1	0.639 (3)	0.6032 (9)	0.4084 (6)	0.038 (3)
O14	0.740 (3)	0.0421 (11)	0.4091 (7)	0.057 (4)
O11	0.759 (3)	0.3822 (9)	0.3549 (6)	0.053 (4)
O13	0.866 (3)	0.1399 (9)	0.4579 (6)	0.043 (5)
O12	0.621 (3)	0.3436 (14)	0.2953 (10)	0.056 (7)
O3	0.571 (3)	1.0085 (8)	0.5868 (6)	0.041 (5)
N13	0.887 (3)	0.2452 (9)	0.2869 (7)	0.036 (5)
H13A	0.9032	0.2616	0.2371	0.037*
H13B	0.9359	0.2261	0.3282	0.037*
H13C	0.8752	0.3250	0.3180	0.037*
O1W	0.581 (3)	0.9885 (13)	0.3074 (7)	0.067 (6)
H1WA	0.635287	0.975314	0.345508	0.101*
H1WB	0.555092	0.951324	0.353999	0.101*
N3	0.46595 (11)	0.82054 (17)	0.56868 (13)	0.033 (6)
H3A	0.4608	0.8449	0.5102	0.044*
H3B	0.4505	0.8821	0.6050	0.044*
H3C	0.4344	0.7541	0.5766	0.044*
O2W	0.500000	0.5268 (14)	0.250000	0.052 (7)
C1	0.578 (5)	0.6751 (13)	0.4467 (8)	0.028 (4)
C4	0.604 (4)	0.8968 (15)	0.5729 (10)	0.024 (5)
C11	0.698 (3)	0.3226 (18)	0.3009 (13)	0.022 (5)
C14	0.810 (5)	0.1117 (13)	0.3958 (9)	0.030 (4)
C12	0.736 (4)	0.2090 (11)	0.2459 (8)	0.032 (4)
H12A	0.746721	0.238171	0.181480	0.038*
H12B	0.693684	0.139348	0.240780	0.038*
C13	0.820 (3)	0.1530 (11)	0.2914 (8)	0.024 (4)
H13	0.835880	0.075561	0.254830	0.029*
C3	0.534 (4)	0.7805 (13)	0.5988 (10)	0.030 (5)
H3	0.535788	0.768394	0.668454	0.036*
C2	0.560 (3)	0.6555 (10)	0.5532 (7)	0.030 (4)
H2A	0.514966	0.591374	0.558842	0.036*
H2B	0.611784	0.622002	0.586690	0.036*
H2W	0.546 (10)	0.474 (14)	0.239 (12)	0.10 (10)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.06 (2)	0.0299 (9)	0.0276 (8)	−0.001 (3)	−0.004 (2)	−0.0006 (6)
O4	0.039 (7)	0.033 (4)	0.044 (5)	−0.004 (5)	0.000 (5)	−0.003 (4)
O2	0.030 (14)	0.037 (4)	0.026 (3)	−0.005 (9)	−0.002 (8)	−0.002 (3)
O1	0.038 (7)	0.043 (4)	0.033 (4)	−0.001 (5)	0.000 (5)	−0.001 (3)
O14	0.056 (8)	0.062 (5)	0.052 (4)	−0.003 (5)	0.003 (5)	0.011 (4)
O11	0.053 (7)	0.050 (4)	0.056 (4)	−0.001 (5)	0.002 (5)	−0.016 (4)
O13	0.042 (14)	0.056 (5)	0.031 (4)	−0.004 (10)	−0.002 (9)	0.001 (4)
O12	0.056 (15)	0.054 (8)	0.058 (7)	0.000 (10)	0.003 (10)	0.001 (5)
O3	0.041 (14)	0.036 (5)	0.046 (4)	−0.001 (9)	−0.002 (10)	−0.004 (4)
N13	0.037 (14)	0.033 (5)	0.037 (5)	−0.003 (10)	0.005 (9)	0.008 (4)
O1W	0.068 (14)	0.054 (5)	0.080 (7)	−0.003 (10)	0.018 (10)	−0.018 (5)
N3	0.033 (14)	0.033 (6)	0.033 (6)	0.001 (10)	0.009 (10)	−0.002 (5)
O2W	0.050 (14)	0.036 (7)	0.067 (7)	0.000	−0.011 (10)	0.000
C1	0.028 (8)	0.030 (5)	0.026 (5)	−0.001 (5)	0.002 (5)	0.000 (4)
C4	0.025 (8)	0.024 (6)	0.025 (5)	0.000 (5)	0.003 (5)	−0.002 (4)
C11	0.022 (8)	0.021 (6)	0.023 (6)	0.000 (5)	0.001 (5)	−0.002 (4)
C14	0.030 (8)	0.029 (5)	0.032 (5)	0.001 (5)	0.000 (5)	−0.001 (4)
C12	0.032 (8)	0.032 (5)	0.031 (5)	−0.001 (5)	0.001 (5)	0.002 (4)
C13	0.024 (7)	0.025 (4)	0.023 (4)	0.001 (5)	0.002 (5)	0.000 (4)
C3	0.030 (8)	0.032 (6)	0.027 (5)	0.000 (5)	0.001 (5)	−0.003 (4)
C2	0.030 (7)	0.031 (4)	0.029 (4)	0.001 (5)	0.001 (5)	0.000 (4)

Geometric parameters (Å, º)

Zn1—O4^i	1.85 (3)	O12—C11	1.21 (6)
Zn1—O1	1.91 (4)	O3—C4	1.27 (3)
Zn1—O14^ii	1.981 (12)	N13—C13	1.410 (13)
Zn1—O11	1.925 (12)	N3—C3	1.19 (5)
Zn1—C14^ii	2.54 (3)	C1—C2	1.54 (2)
O4—C4	1.34 (6)	C4—C3	1.66 (6)
O2—C1	1.22 (4)	C11—C12	1.53 (4)
O1—C1	1.33 (7)	C14—C13	1.533 (19)
O14—C14	1.32 (7)	C12—C13	1.54 (6)
O11—C11	1.33 (5)	C3—C2	1.49 (3)
O13—C14	1.23 (6)
O4^i—Zn1—O1	97.8 (14)	O3—C4—C3	110 (4)
O4^i—Zn1—O14^ii	96.9 (11)	O11—C11—C12	111 (4)
O4^i—Zn1—O11	108.8 (13)	O12—C11—O11	129 (3)
O4^i—Zn1—C14^ii	126.3 (11)	O12—C11—C12	120 (3)
O1—Zn1—O14^ii	124.3 (13)	O14—C14—Zn1^ii	50.3 (10)
O1—Zn1—O11	105.0 (10)	O14—C14—C13	114 (3)
O1—Zn1—C14^ii	105.7 (13)	O13—C14—Zn1^ii	75.6 (13)
O14^ii—Zn1—C14^ii	30.8 (17)	O13—C14—O14	126 (2)
O11—Zn1—O14^ii	120.1 (7)	O13—C14—C13	120 (5)
O11—Zn1—C14^ii	110.4 (5)	C13—C14—Zn1^ii	163 (3)
C4—O4—Zn1^i	115.7 (14)	C11—C12—C13	115 (2)
C1—O1—Zn1	136.3 (16)	N13—C13—C14	110 (2)
C14—O14—Zn1^ii	99 (2)	N13—C13—C12	110.5 (17)
C11—O11—Zn1	125 (3)	C14—C13—C12	112 (4)
O2—C1—O1	123.1 (19)	N3—C3—C4	104.9 (18)
O2—C1—C2	118 (4)	N3—C3—C2	112 (3)
O1—C1—C2	119 (3)	C2—C3—C4	109 (4)
O4—C4—C3	118 (2)	C3—C2—C1	111.5 (13)
O3—C4—O4	132 (4)
O2—C1—C2—C3	−31 (6)	C1—C2—C3—N3	72 (5)
O12—C11—C12—C13	−153 (3)	C1—C2—C3—C4	−49 (5)
N13—C13—C14—O13	−13 (4)	C11—C12—C13—N13	−67 (3)
N3—C3—C4—O3	38 (2)	C11—C12—C13—C14	55 (3)

Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+3/2, −y+1/2, −z+1.

(Zn-aspartate_dihydrate_0_001GPa)

Crystal data

C16H24N4O16Zn2·4(H2O)	Z = 1
Mr = 731.19	F(000) = 376
Triclinic, P1	Dx = 1.857 Mg m^−3
a = 8.7873 (3) Å	Cu Kα radiation, λ = 1.54184 Å
b = 9.5061 (3) Å	Cell parameters from 2677 reflections
c = 9.8114 (3) Å	θ = 5.4–76.3°
α = 111.784 (3)°	µ = 3.18 mm^−1
β = 105.625 (3)°	T = 296 K
γ = 107.721 (3)°	Plate, colourless
V = 653.73 (4) Å^3	0.25 × 0.10 × 0.02 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.020
Radiation source: sealed x-ray tube	θmax = 76.3°, θmin = 5.4°
ω scan	h = −11→9
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −11→11
Tmin = 0.717, Tmax = 0.938	l = −12→12
13265 measured reflections	150 standard reflections every 26 reflections
2706 independent reflections	intensity decay: none
2677 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Hydrogen site location: mixed
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.024	w = 1/[σ^2(Fo^2) + (0.0323P)^2 + 0.3903P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.065	(Δ/σ)max < 0.001
S = 1.09	Δρmax = 0.36 e Å^−3
2706 reflections	Δρmin = −0.38 e Å^−3
199 parameters	Extinction correction: SHELXL-2017/1 (Sheldrick 2017), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0057 (5)
Primary atom site location: dual

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.71338 (3)	0.32287 (3)	0.54502 (2)	0.02403 (10)
O1	0.64345 (16)	0.34223 (15)	0.72174 (14)	0.0283 (3)
O2	0.57225 (16)	0.27339 (15)	0.89453 (14)	0.0298 (3)
O14	1.10055 (15)	0.75024 (16)	0.46798 (14)	0.0310 (3)
O4	0.50319 (16)	−0.11786 (15)	0.63065 (14)	0.0324 (3)
O11	0.72596 (19)	0.50154 (16)	0.49431 (15)	0.0378 (3)
O1W	0.23254 (17)	0.02884 (16)	0.77486 (16)	0.0345 (3)
H1WA	0.340238	0.092262	0.803331	0.052*
H1WB	0.196709	−0.048038	0.677750	0.052*
O13	0.92845 (17)	0.50309 (17)	0.24279 (17)	0.0388 (3)
O3	0.50923 (18)	−0.16090 (16)	0.84088 (15)	0.0374 (3)
O12	0.84265 (19)	0.73004 (18)	0.73867 (15)	0.0392 (3)
O2W	0.2269 (2)	0.3194 (2)	1.0024 (2)	0.0511 (4)
H2WA	0.218738	0.220466	0.954567	0.077*
H2WB	0.218624	0.329127	1.089515	0.077*
N13	0.62832 (18)	0.52692 (19)	0.21564 (17)	0.0290 (3)
H13A	0.636167	0.482799	0.121891	0.035*
H13B	0.539355	0.554456	0.201408	0.035*
H13C	0.608602	0.450977	0.249310	0.035*
N3	0.7820 (2)	0.15150 (18)	1.05345 (17)	0.0315 (3)
H3A	0.711687	0.201226	1.064078	0.038*
H3B	0.894515	0.228842	1.117093	0.038*
H3C	0.756227	0.072026	1.082374	0.038*
C1	0.6580 (2)	0.27527 (19)	0.81203 (18)	0.0221 (3)
C4	0.5710 (2)	−0.08268 (19)	0.77797 (19)	0.0241 (3)
C14	0.9503 (2)	0.6363 (2)	0.34881 (19)	0.0242 (3)
C11	0.7887 (2)	0.6605 (2)	0.5899 (2)	0.0258 (3)
C12	0.7913 (2)	0.7641 (2)	0.5036 (2)	0.0254 (3)
H12A	0.893776	0.874522	0.573857	0.030*
H12B	0.686412	0.782128	0.486345	0.030*
C13	0.7974 (2)	0.6821 (2)	0.34022 (19)	0.0246 (3)
H13	0.812732	0.764412	0.301412	0.030*
C2	0.7876 (2)	0.2006 (2)	0.8223 (2)	0.0269 (3)
H2A	0.906071	0.292826	0.894831	0.032*
H2B	0.783972	0.146034	0.715300	0.032*
C3	0.7547 (2)	0.0723 (2)	0.88178 (19)	0.0255 (3)
H3	0.842687	0.029647	0.877107	0.031*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.02528 (14)	0.02665 (14)	0.02281 (13)	0.01219 (10)	0.01190 (9)	0.01326 (10)
O1	0.0353 (6)	0.0368 (6)	0.0263 (6)	0.0222 (5)	0.0178 (5)	0.0202 (5)
O2	0.0316 (6)	0.0341 (6)	0.0289 (6)	0.0148 (5)	0.0188 (5)	0.0165 (5)
O14	0.0223 (6)	0.0341 (6)	0.0282 (6)	0.0119 (5)	0.0094 (5)	0.0092 (5)
O4	0.0299 (6)	0.0323 (6)	0.0234 (6)	0.0074 (5)	0.0057 (5)	0.0122 (5)
O11	0.0543 (8)	0.0268 (6)	0.0269 (6)	0.0146 (6)	0.0125 (6)	0.0146 (5)
O1W	0.0346 (7)	0.0313 (6)	0.0325 (6)	0.0120 (5)	0.0140 (5)	0.0135 (5)
O13	0.0314 (7)	0.0322 (6)	0.0400 (7)	0.0165 (5)	0.0125 (6)	0.0063 (6)
O3	0.0388 (7)	0.0317 (6)	0.0315 (6)	0.0039 (5)	0.0167 (6)	0.0146 (5)
O12	0.0483 (8)	0.0427 (7)	0.0243 (6)	0.0203 (6)	0.0155 (6)	0.0147 (6)
O2W	0.0637 (10)	0.0519 (9)	0.0422 (8)	0.0319 (8)	0.0263 (8)	0.0206 (7)
N13	0.0249 (7)	0.0367 (8)	0.0236 (7)	0.0167 (6)	0.0075 (5)	0.0132 (6)
N3	0.0357 (8)	0.0251 (7)	0.0240 (7)	0.0089 (6)	0.0059 (6)	0.0119 (6)
C1	0.0213 (7)	0.0206 (7)	0.0189 (7)	0.0062 (6)	0.0073 (6)	0.0083 (6)
C4	0.0239 (7)	0.0233 (7)	0.0237 (7)	0.0109 (6)	0.0110 (6)	0.0098 (6)
C14	0.0239 (8)	0.0283 (8)	0.0249 (7)	0.0123 (6)	0.0125 (6)	0.0155 (6)
C11	0.0237 (7)	0.0298 (8)	0.0256 (8)	0.0129 (6)	0.0116 (6)	0.0139 (7)
C12	0.0263 (8)	0.0247 (7)	0.0270 (8)	0.0140 (6)	0.0122 (6)	0.0121 (6)
C13	0.0265 (8)	0.0265 (7)	0.0251 (7)	0.0136 (6)	0.0113 (6)	0.0153 (6)
C2	0.0237 (8)	0.0300 (8)	0.0333 (8)	0.0126 (7)	0.0140 (7)	0.0199 (7)
C3	0.0245 (8)	0.0257 (8)	0.0249 (8)	0.0102 (6)	0.0087 (6)	0.0136 (6)

Geometric parameters (Å, º)

Zn1—O1	1.9555 (11)	N13—H13C	0.8900
Zn1—O14^i	1.9776 (12)	N13—C13	1.492 (2)
Zn1—O4^ii	1.9679 (12)	N3—H3A	0.8900
Zn1—O11	1.9203 (13)	N3—H3B	0.8900
O1—C1	1.2701 (19)	N3—H3C	0.8900
O2—C1	1.2465 (19)	N3—C3	1.481 (2)
O14—C14	1.281 (2)	C1—C2	1.515 (2)
O4—C4	1.270 (2)	C4—C3	1.538 (2)
O11—C11	1.276 (2)	C14—C13	1.524 (2)
O1W—H1WA	0.8499	C11—C12	1.518 (2)
O1W—H1WB	0.8500	C12—H12A	0.9700
O13—C14	1.220 (2)	C12—H12B	0.9700
O3—C4	1.226 (2)	C12—C13	1.525 (2)
O12—C11	1.230 (2)	C13—H13	0.9800
O2W—H2WA	0.8500	C2—H2A	0.9700
O2W—H2WB	0.8504	C2—H2B	0.9700
N13—H13A	0.8900	C2—C3	1.522 (2)
N13—H13B	0.8900	C3—H3	0.9800
O1—Zn1—O14^i	119.50 (5)	O14—C14—C13	115.30 (14)
O1—Zn1—O4^ii	96.87 (5)	O13—C14—O14	123.85 (15)
O4^ii—Zn1—O14^i	102.06 (5)	O13—C14—C13	120.73 (15)
O11—Zn1—O1	113.53 (5)	O11—C11—C12	113.83 (14)
O11—Zn1—O14^i	114.64 (6)	O12—C11—O11	125.68 (16)
O11—Zn1—O4^ii	106.77 (5)	O12—C11—C12	120.49 (15)
C1—O1—Zn1	131.64 (11)	C11—C12—H12A	108.7
C14—O14—Zn1^i	110.34 (10)	C11—C12—H12B	108.7
C4—O4—Zn1^ii	125.56 (11)	C11—C12—C13	114.04 (13)
C11—O11—Zn1	129.48 (11)	H12A—C12—H12B	107.6
H1WA—O1W—H1WB	104.5	C13—C12—H12A	108.7
H2WA—O2W—H2WB	104.4	C13—C12—H12B	108.7
H13A—N13—H13B	109.5	N13—C13—C14	108.61 (13)
H13A—N13—H13C	109.5	N13—C13—C12	111.84 (13)
H13B—N13—H13C	109.5	N13—C13—H13	107.4
C13—N13—H13A	109.5	C14—C13—C12	114.03 (13)
C13—N13—H13B	109.5	C14—C13—H13	107.3
C13—N13—H13C	109.5	C12—C13—H13	107.4
H3A—N3—H3B	109.5	C1—C2—H2A	108.5
H3A—N3—H3C	109.5	C1—C2—H2B	108.5
H3B—N3—H3C	109.5	C1—C2—C3	115.28 (13)
C3—N3—H3A	109.5	H2A—C2—H2B	107.5
C3—N3—H3B	109.5	C3—C2—H2A	108.5
C3—N3—H3C	109.5	C3—C2—H2B	108.5
O1—C1—C2	118.45 (14)	N3—C3—C4	108.71 (13)
O2—C1—O1	121.88 (15)	N3—C3—C2	111.96 (13)
O2—C1—C2	119.64 (14)	N3—C3—H3	107.1
O4—C4—C3	113.75 (14)	C4—C3—H3	107.1
O3—C4—O4	127.36 (16)	C2—C3—C4	114.55 (13)
O3—C4—C3	118.84 (14)	C2—C3—H3	107.1
Zn1—O1—C1—C2	17.6 (2)	N13—C13—C14—O13	14.0 (2)
Zn1—O14^i—C14^i—C13^i	176.84 (10)	N3—C3—C4—O3	−29.7 (2)
Zn1—O4^ii—C4^ii—C3^ii	−171.30 (10)	C1—C2—C3—N3	−65.97 (18)
Zn1—O11—C11—C12	174.20 (12)	C1—C2—C3—C4	58.40 (19)
O2—C1—C2—C3	22.0 (2)	C11—C12—C13—N13	69.02 (17)
O12—C11—C12—C13	155.34 (16)	C11—C12—C13—C14	−54.71 (18)

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

(Zn-aspartate_dihydrate_0_05GPa)

Crystal data

C16H24N4O16Zn2·4(H2O)	Z = 1
Mr = 731.19	F(000) = 376
Triclinic, P1	Dx = 1.862 Mg m^−3
a = 8.7874 (12) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.4894 (15) Å	Cell parameters from 393 reflections
c = 9.812 (3) Å	θ = 3.8–27.3°
α = 111.913 (19)°	µ = 1.94 mm^−1
β = 105.549 (16)°	T = 296 K
γ = 107.728 (13)°	Plate, colourless
V = 652.1 (2) Å^3	0.25 × 0.20 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.052
Radiation source: sealed x-ray tube	θmax = 27.3°, θmin = 3.8°
ω scan	h = −11→10
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −11→12
Tmin = 0.634, Tmax = 0.925	l = −7→7
2655 measured reflections	12 standard reflections every 84 reflections
479 independent reflections	intensity decay: none
393 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.046	H-atom parameters constrained
wR(F^2) = 0.135	w = 1/[σ^2(Fo^2) + (0.1035P)^2 + 1.095P] where P = (Fo^2 + 2Fc^2)/3
S = 1.12	(Δ/σ)max < 0.001
479 reflections	Δρmax = 0.28 e Å^−3
198 parameters	Δρmin = −0.32 e Å^−3
132 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 0.05 (2) GPa (50000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7142 (3)	0.3234 (5)	0.5464 (8)	0.028 (2)
O1	0.646 (2)	0.346 (4)	0.725 (5)	0.028 (3)
O2	0.5698 (18)	0.270 (3)	0.890 (5)	0.033 (5)
O14	1.1008 (19)	0.753 (3)	0.473 (5)	0.033 (3)
O4	0.501 (2)	−0.120 (3)	0.621 (5)	0.044 (4)
O11	0.7272 (19)	0.502 (3)	0.498 (5)	0.050 (4)
O1W	0.229 (3)	0.028 (3)	0.773 (5)	0.039 (5)
H1WA	0.339706	0.090904	0.823655	0.058*
H1WB	0.214100	−0.047681	0.682640	0.058*
O13	0.9263 (17)	0.500 (3)	0.238 (4)	0.043 (5)
O3	0.5090 (18)	−0.161 (3)	0.842 (4)	0.043 (5)
O12	0.841 (2)	0.727 (4)	0.733 (5)	0.043 (7)
O2W	0.225 (2)	0.318 (4)	1.003 (6)	0.066 (6)
H2WA	0.247907	0.235171	0.963035	0.098*
H2WB	0.176532	0.296431	1.061845	0.098*
N13	0.626 (2)	0.523 (4)	0.211 (6)	0.030 (5)
H13A	0.636167	0.482799	0.121891	0.035*
H13B	0.539355	0.554456	0.201408	0.035*
H13C	0.608602	0.450977	0.249310	0.035*
N3	0.778 (2)	0.146 (3)	1.042 (5)	0.031 (6)
H3A	0.711687	0.201226	1.064078	0.038*
H3B	0.894515	0.228842	1.117093	0.038*
H3C	0.756227	0.072026	1.082374	0.038*
C1	0.655 (3)	0.273 (4)	0.807 (7)	0.027 (4)
C4	0.564 (2)	−0.085 (3)	0.770 (5)	0.026 (4)
C14	0.949 (2)	0.638 (4)	0.351 (5)	0.027 (4)
C11	0.786 (3)	0.659 (3)	0.586 (5)	0.039 (7)
C12	0.787 (2)	0.759 (4)	0.494 (6)	0.018 (4)
H12A	0.679509	0.772511	0.473034	0.022*
H12B	0.886233	0.871361	0.564684	0.022*
C13	0.799 (2)	0.681 (4)	0.337 (6)	0.022 (4)
H13	0.815194	0.763133	0.298392	0.026*
C2	0.786 (3)	0.195 (5)	0.815 (7)	0.025 (4)
H2A	0.779628	0.138528	0.707446	0.030*
H2B	0.905045	0.287191	0.886078	0.030*
C3	0.754 (2)	0.071 (3)	0.876 (5)	0.036 (6)
H3	0.840650	0.026723	0.869972	0.043*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0274 (14)	0.032 (3)	0.025 (6)	0.0136 (16)	0.012 (2)	0.015 (4)
O1	0.028 (3)	0.031 (5)	0.028 (7)	0.015 (3)	0.013 (4)	0.013 (5)
O2	0.036 (5)	0.039 (8)	0.030 (13)	0.017 (5)	0.018 (7)	0.018 (9)
O14	0.030 (4)	0.033 (5)	0.034 (7)	0.015 (3)	0.015 (4)	0.013 (5)
O4	0.047 (5)	0.041 (6)	0.044 (7)	0.016 (3)	0.018 (4)	0.024 (5)
O11	0.057 (5)	0.047 (5)	0.049 (7)	0.021 (3)	0.018 (4)	0.032 (5)
O1W	0.039 (5)	0.035 (9)	0.040 (13)	0.015 (5)	0.019 (7)	0.016 (9)
O13	0.033 (5)	0.049 (9)	0.043 (13)	0.021 (5)	0.015 (7)	0.017 (9)
O3	0.045 (5)	0.043 (8)	0.040 (13)	0.012 (5)	0.021 (7)	0.023 (9)
O12	0.043 (7)	0.047 (9)	0.041 (14)	0.020 (6)	0.019 (8)	0.023 (9)
O2W	0.066 (7)	0.063 (9)	0.066 (13)	0.033 (6)	0.025 (8)	0.030 (9)
N13	0.031 (5)	0.031 (9)	0.029 (13)	0.017 (5)	0.013 (7)	0.013 (9)
N3	0.037 (6)	0.025 (9)	0.033 (13)	0.015 (5)	0.016 (8)	0.016 (9)
C1	0.026 (5)	0.025 (5)	0.028 (7)	0.009 (3)	0.012 (4)	0.013 (5)
C4	0.026 (5)	0.023 (6)	0.026 (7)	0.009 (4)	0.007 (5)	0.015 (5)
C14	0.026 (5)	0.027 (6)	0.027 (7)	0.012 (4)	0.011 (4)	0.012 (5)
C11	0.040 (8)	0.038 (8)	0.040 (10)	0.020 (5)	0.015 (5)	0.019 (6)
C12	0.019 (5)	0.019 (5)	0.018 (7)	0.010 (4)	0.007 (4)	0.010 (5)
C13	0.022 (5)	0.024 (6)	0.021 (7)	0.009 (4)	0.011 (4)	0.012 (5)
C2	0.026 (4)	0.024 (5)	0.025 (7)	0.011 (3)	0.010 (4)	0.013 (5)
C3	0.036 (6)	0.036 (7)	0.035 (8)	0.016 (4)	0.016 (5)	0.018 (6)

Geometric parameters (Å, º)

Zn1—O1	1.96 (4)	N13—H13C	0.8900
Zn1—O14^i	1.993 (14)	N13—C13	1.52 (4)
Zn1—O4^ii	1.93 (3)	N3—H3A	0.9100
Zn1—O11	1.909 (9)	N3—H3B	0.9400
O1—C1	1.25 (3)	N3—H3C	0.9100
O2—C1	1.25 (4)	N3—C3	1.44 (3)
O14—C14	1.29 (4)	C1—C2	1.54 (2)
O4—C4	1.28 (4)	C4—C3	1.58 (3)
O11—C11	1.25 (3)	C14—C13	1.49 (2)
O1W—H1WA	0.8498	C11—C12	1.53 (4)
O1W—H1WB	0.8484	C12—H12A	0.9700
O13—C14	1.27 (2)	C12—H12B	0.9700
O3—C4	1.27 (3)	C12—C13	1.49 (3)
O12—C11	1.21 (4)	C13—H13	0.9800
O2W—H2WA	0.8476	C2—H2A	0.9700
O2W—H2WB	0.8501	C2—H2B	0.9700
N13—H13A	0.8600	C2—C3	1.49 (3)
N13—H13B	0.8900	C3—H3	0.9800
O1—Zn1—O14^i	120.9 (9)	O14—C14—C13	116 (3)
O4^ii—Zn1—O1	95.6 (10)	O13—C14—O14	124.4 (18)
O4^ii—Zn1—O14^i	101.7 (11)	O13—C14—C13	119 (2)
O11—Zn1—O1	112.7 (11)	O11—C11—C12	114 (3)
O11—Zn1—O14^i	114.2 (6)	O12—C11—O11	123 (3)
O11—Zn1—O4^ii	108.3 (11)	O12—C11—C12	123 (3)
C1—O1—Zn1	130 (2)	C11—C12—H12A	108.3
C14—O14—Zn1^i	109 (2)	C11—C12—H12B	108.3
C4—O4—Zn1^ii	122.7 (11)	H12A—C12—H12B	107.4
C11—O11—Zn1	132 (3)	C13—C12—C11	116 (2)
H1WA—O1W—H1WB	104.4	C13—C12—H12A	108.3
H2WA—O2W—H2WB	104.4	C13—C12—H12B	108.3
H13A—N13—H13B	112.0	N13—C13—H13	107.8
H13A—N13—H13C	113.0	C14—C13—N13	110 (2)
H13B—N13—H13C	109.5	C14—C13—C12	114 (2)
C13—N13—H13A	107.0	C14—C13—H13	107.8
C13—N13—H13B	108.0	C12—C13—N13	110 (2)
C13—N13—H13C	107.0	C12—C13—H13	107.8
H3A—N3—H3B	104.0	C1—C2—H2A	108.6
H3A—N3—H3C	105.0	C1—C2—H2B	108.6
H3B—N3—H3C	102.0	H2A—C2—H2B	107.5
C3—N3—H3A	115.0	C3—C2—C1	115 (2)
C3—N3—H3B	114.0	C3—C2—H2A	108.6
C3—N3—H3C	116.0	C3—C2—H2B	108.6
O1—C1—C2	119 (3)	N3—C3—C4	107 (2)
O2—C1—O1	121.5 (17)	N3—C3—C2	114 (3)
O2—C1—C2	120 (2)	N3—C3—H3	107.4
O4—C4—C3	113 (2)	C4—C3—H3	107.4
O3—C4—O4	132 (2)	C2—C3—C4	113 (3)
O3—C4—C3	115 (3)	C2—C3—H3	107.4
Zn1—O1—C1—C2	21 (6)	N13—C13—C14—O13	17 (3)
Zn1—O14^i—C14^i—C13^i	174.3 (16)	N3—C3—C4—O3	−31 (2)
Zn1—O4^ii—C4^ii—C3^ii	−171.0 (15)	C1—C2—C3—N3	−64 (4)
Zn1—O11—C11—C12	173.9 (10)	C1—C2—C3—C4	59 (6)
O2—C1—C2—C3	20 (7)	C11—C12—C13—N13	70.8 (16)
O12—C11—C12—C13	152 (2)	C11—C12—C13—C14	−52.7 (17)

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

(Zn-aspartate_dihydrate_0_15GPa)

Crystal data

C16H24N4O16Zn2·4(H2O)	Z = 1
Mr = 731.19	F(000) = 376
Triclinic, P1	Dx = 1.871 Mg m^−3
a = 8.7725 (11) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.4694 (14) Å	Cell parameters from 389 reflections
c = 9.803 (3) Å	θ = 3.8–27.2°
α = 111.906 (19)°	µ = 1.95 mm^−1
β = 105.503 (16)°	T = 296 K
γ = 107.777 (12)°	Plate, colourless
V = 649.0 (2) Å^3	0.25 × 0.20 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.068
Radiation source: sealed x-ray tube	θmax = 27.2°, θmin = 3.8°
ω scan	h = −10→10
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −11→12
Tmin = 0.633, Tmax = 0.907	l = −7→7
2630 measured reflections	12 standard reflections every 84 reflections
474 independent reflections	intensity decay: none
389 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.052	H-atom parameters constrained
wR(F^2) = 0.129	w = 1/[σ^2(Fo^2) + (0.0808P)^2 + 2.3162P] where P = (Fo^2 + 2Fc^2)/3
S = 1.13	(Δ/σ)max < 0.001
474 reflections	Δρmax = 0.28 e Å^−3
198 parameters	Δρmin = −0.27 e Å^−3
132 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 0.15 (2) GPa (150000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7133 (3)	0.3224 (4)	0.5446 (7)	0.0281 (19)
O1	0.642 (2)	0.339 (3)	0.713 (5)	0.028 (3)
O2	0.5696 (16)	0.270 (3)	0.886 (4)	0.031 (4)
O14	1.1038 (18)	0.759 (3)	0.481 (4)	0.029 (3)
O4	0.503 (2)	−0.120 (3)	0.620 (4)	0.043 (4)
O11	0.7231 (16)	0.496 (2)	0.485 (3)	0.047 (3)
O1W	0.228 (2)	0.024 (3)	0.767 (4)	0.030 (4)
H1WA	0.3362	0.0949	0.8293	0.045*
H1WB	0.2302	−0.0545	0.6901	0.045*
O13	0.9257 (16)	0.500 (3)	0.236 (4)	0.036 (4)
O3	0.5115 (16)	−0.161 (3)	0.844 (4)	0.043 (4)
O12	0.841 (2)	0.735 (3)	0.738 (4)	0.047 (6)
O2W	0.2233 (19)	0.315 (3)	0.999 (5)	0.063 (5)
H2WA	0.2547	0.2434	0.9616	0.095*
H2WB	0.1757	0.2884	1.0585	0.095*
N13	0.629 (2)	0.525 (4)	0.216 (5)	0.032 (4)
H13A	0.636167	0.482799	0.121891	0.035*
H13B	0.539355	0.554456	0.201408	0.035*
H13C	0.608602	0.450977	0.249310	0.035*
N3	0.7811 (19)	0.155 (3)	1.054 (5)	0.032 (5)
H3A	0.711687	0.201226	1.064078	0.038*
H3B	0.894515	0.228842	1.117093	0.038*
H3C	0.756227	0.072026	1.082374	0.038*
C1	0.656 (2)	0.274 (4)	0.808 (6)	0.026 (3)
C4	0.564 (2)	−0.083 (3)	0.777 (4)	0.026 (4)
C14	0.956 (2)	0.646 (3)	0.365 (5)	0.020 (4)
C11	0.790 (3)	0.659 (3)	0.594 (4)	0.038 (7)
C12	0.7920 (19)	0.768 (3)	0.510 (5)	0.025 (4)
H12A	0.8947	0.8786	0.5814	0.031*
H12B	0.6868	0.7853	0.4942	0.031*
C13	0.7979 (18)	0.686 (3)	0.344 (5)	0.022 (4)
H13	0.8146	0.7691	0.3054	0.026*
C2	0.789 (2)	0.202 (4)	0.827 (7)	0.026 (3)
H2A	0.7947	0.1536	0.7231	0.031*
H2B	0.9048	0.2969	0.9054	0.031*
C3	0.756 (2)	0.070 (3)	0.878 (5)	0.036 (5)
H3	0.8429	0.0251	0.8723	0.044*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0273 (12)	0.029 (2)	0.030 (5)	0.0132 (14)	0.015 (2)	0.015 (3)
O1	0.029 (3)	0.031 (4)	0.027 (6)	0.014 (3)	0.015 (4)	0.015 (4)
O2	0.035 (4)	0.033 (7)	0.029 (11)	0.014 (4)	0.022 (6)	0.015 (8)
O14	0.028 (3)	0.033 (4)	0.027 (6)	0.011 (3)	0.014 (4)	0.015 (4)
O4	0.044 (4)	0.039 (5)	0.043 (6)	0.012 (3)	0.019 (4)	0.023 (5)
O11	0.055 (4)	0.043 (4)	0.046 (6)	0.020 (3)	0.015 (4)	0.031 (4)
O1W	0.034 (5)	0.039 (7)	0.022 (11)	0.012 (4)	0.018 (6)	0.020 (8)
O13	0.037 (5)	0.046 (8)	0.032 (11)	0.021 (5)	0.017 (6)	0.022 (8)
O3	0.043 (5)	0.041 (7)	0.045 (11)	0.012 (4)	0.024 (6)	0.022 (8)
O12	0.046 (7)	0.048 (8)	0.046 (12)	0.021 (5)	0.026 (7)	0.019 (8)
O2W	0.063 (6)	0.065 (8)	0.063 (11)	0.032 (5)	0.028 (7)	0.031 (8)
N13	0.029 (5)	0.031 (8)	0.035 (11)	0.017 (5)	0.016 (7)	0.011 (8)
N3	0.035 (6)	0.034 (8)	0.030 (12)	0.015 (5)	0.016 (7)	0.019 (8)
C1	0.025 (4)	0.025 (5)	0.026 (6)	0.010 (3)	0.010 (4)	0.013 (4)
C4	0.030 (5)	0.024 (5)	0.025 (7)	0.006 (3)	0.011 (4)	0.017 (5)
C14	0.023 (4)	0.020 (5)	0.018 (6)	0.005 (3)	0.010 (4)	0.013 (5)
C11	0.037 (8)	0.037 (8)	0.038 (9)	0.019 (5)	0.014 (5)	0.018 (6)
C12	0.026 (5)	0.026 (5)	0.025 (7)	0.012 (4)	0.010 (4)	0.014 (5)
C13	0.023 (4)	0.023 (5)	0.021 (6)	0.008 (3)	0.012 (4)	0.012 (5)
C2	0.024 (4)	0.025 (5)	0.027 (6)	0.011 (3)	0.012 (4)	0.011 (4)
C3	0.035 (6)	0.036 (6)	0.037 (7)	0.015 (4)	0.018 (4)	0.017 (5)

Geometric parameters (Å, º)

Zn1—O1	1.89 (4)	N13—H13C	0.8700
Zn1—O14^i	2.013 (15)	N13—C13	1.51 (5)
Zn1—O4^ii	1.92 (3)	N3—H3A	0.8600
Zn1—O11	1.924 (10)	N3—H3B	0.8900
O1—C1	1.29 (4)	N3—H3C	0.9100
O2—C1	1.22 (4)	N3—C3	1.52 (3)
O14—C14	1.25 (4)	C1—C2	1.520 (19)
O4—C4	1.344 (13)	C4—C3	1.57 (3)
O11—C11	1.321 (13)	C14—C13	1.53 (2)
O1W—H1WA	0.8501	C11—C12	1.54 (4)
O1W—H1WB	0.8501	C12—H12A	0.9700
O13—C14	1.37 (3)	C12—H12B	0.9700
O3—C4	1.24 (3)	C12—C13	1.55 (3)
O12—C11	1.20 (3)	C13—H13	0.9800
O2W—H2WA	0.8101	C2—H2A	0.9700
O2W—H2WB	0.8726	C2—H2B	0.9700
N13—H13A	0.8900	C2—C3	1.50 (3)
N13—H13B	0.9100	C3—H3	0.9800
O1—Zn1—O14^i	122.1 (10)	O14—C14—O13	126.3 (19)
O1—Zn1—O4^ii	93.3 (11)	O14—C14—C13	119 (3)
O1—Zn1—O11	115.6 (10)	O13—C14—C13	114 (3)
O4^ii—Zn1—O14^i	101.2 (11)	O11—C11—C12	111 (3)
O11—Zn1—O14^i	113.1 (6)	O12—C11—O11	134 (3)
O11—Zn1—O4^ii	106.5 (10)	O12—C11—C12	116 (3)
C1—O1—Zn1	133 (2)	C11—C12—H12A	108.9
C14—O14—Zn1^i	108 (2)	C11—C12—H12B	108.9
C4—O4—Zn1^ii	121.2 (12)	C11—C12—C13	113 (2)
C11—O11—Zn1	122.9 (19)	H12A—C12—H12B	107.7
H1WA—O1W—H1WB	104.5	C13—C12—H12A	108.9
H2WA—O2W—H2WB	105.4	C13—C12—H12B	108.9
H13A—N13—H13B	108.0	N13—C13—C14	110 (3)
H13A—N13—H13C	112.0	N13—C13—C12	113 (2)
H13B—N13—H13C	110.0	N13—C13—H13	108.2
C13—N13—H13A	109.5	C14—C13—C12	110 (3)
C13—N13—H13B	107.0	C14—C13—H13	108.2
C13—N13—H13C	109.5	C12—C13—H13	108.2
H3A—N3—H3B	113.0	C1—C2—H2A	107.8
H3A—N3—H3C	109.5	C1—C2—H2B	107.8
H3B—N3—H3C	107.0	H2A—C2—H2B	107.1
C3—N3—H3A	111.0	C3—C2—C1	118.1 (18)
C3—N3—H3B	108.0	C3—C2—H2A	107.8
C3—N3—H3C	107.0	C3—C2—H2B	107.8
O1—C1—C2	119 (3)	N3—C3—C4	106 (2)
O2—C1—O1	122.9 (15)	N3—C3—H3	109.2
O2—C1—C2	118 (3)	C4—C3—H3	109.2
O4—C4—C3	111 (2)	C2—C3—N3	108 (3)
O3—C4—O4	132 (2)	C2—C3—C4	114 (3)
O3—C4—C3	116 (3)	C2—C3—H3	109.2
Zn1—O1—C1—C2	17 (6)	N13—C13—C14—O13	20 (3)
Zn1—O14^i—C14^i—C13^i	172.6 (18)	N3—C3—C4—O3	−37 (3)
Zn1—O4^ii—C4^ii—C3^ii	−170.4 (15)	C1—C2—C3—N3	−68 (5)
Zn1—O11—C11—C12	175.8 (11)	C1—C2—C3—C4	50 (6)
O2—C1—C2—C3	25 (7)	C11—C12—C13—N13	67.7 (17)
O12—C11—C12—C13	157 (2)	C11—C12—C13—C14	−54.9 (17)

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

(Zn-aspartate_dihydrate_0_40GPa)

Crystal data

C16H24N4O16Zn2·4(H2O)	Z = 1
Mr = 731.19	F(000) = 376
Triclinic, P1	Dx = 1.893 Mg m^−3
a = 8.7385 (18) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.419 (3) Å	Cell parameters from 380 reflections
c = 9.773 (6) Å	θ = 3.8–27.3°
α = 111.86 (4)°	µ = 1.97 mm^−1
β = 105.42 (3)°	T = 296 K
γ = 107.88 (2)°	Plate, colourless
V = 641.4 (5) Å^3	0.25 × 0.20 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.065
Radiation source: sealed x-ray tube	θmax = 27.3°, θmin = 3.8°
ω scan	h = −11→10
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −11→12
Tmin = 0.629, Tmax = 0.906	l = −7→7
2596 measured reflections	12 standard reflections every 84 reflections
475 independent reflections	intensity decay: none
380 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.040	H-atom parameters constrained
wR(F^2) = 0.102	w = 1/[σ^2(Fo^2) + (0.0705P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.10	(Δ/σ)max < 0.001
475 reflections	Δρmax = 0.20 e Å^−3
198 parameters	Δρmin = −0.17 e Å^−3
131 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 0.40 (2) GPa (400000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7121 (2)	0.3223 (4)	0.5440 (6)	0.030 (2)
O1	0.6420 (18)	0.341 (3)	0.719 (5)	0.030 (3)
O2	0.5713 (15)	0.270 (2)	0.887 (4)	0.035 (5)
O14	1.1015 (16)	0.753 (3)	0.468 (4)	0.034 (3)
O4	0.5021 (19)	−0.119 (2)	0.622 (4)	0.040 (4)
O11	0.7235 (15)	0.499 (2)	0.488 (4)	0.051 (3)
O1W	0.2286 (16)	0.025 (3)	0.768 (4)	0.035 (5)
H1WA	0.339724	0.079933	0.820061	0.053*
H1WB	0.210666	−0.081387	0.719158	0.053*
O13	0.9266 (17)	0.497 (3)	0.234 (4)	0.041 (5)
O3	0.5108 (14)	−0.162 (2)	0.844 (3)	0.040 (5)
O12	0.843 (2)	0.736 (3)	0.744 (4)	0.055 (7)
O2W	0.2232 (17)	0.316 (3)	0.999 (4)	0.061 (5)
H2WA	0.241624	0.231646	0.954198	0.092*
H2WB	0.178228	0.294249	1.060455	0.092*
N13	0.6287 (19)	0.527 (3)	0.215 (5)	0.031 (5)
H13A	0.636167	0.482799	0.121891	0.035*
H13B	0.539355	0.554456	0.201408	0.035*
H13C	0.608602	0.450977	0.249310	0.035*
N3	0.782 (2)	0.150 (3)	1.049 (4)	0.037 (6)
H3A	0.711687	0.201226	1.064078	0.038*
H3B	0.894515	0.228842	1.117093	0.038*
H3C	0.756227	0.072026	1.082374	0.038*
C1	0.657 (2)	0.272 (4)	0.804 (6)	0.027 (3)
C4	0.5680 (18)	−0.082 (2)	0.776 (4)	0.020 (4)
C14	0.954 (2)	0.641 (4)	0.356 (6)	0.024 (4)
C11	0.791 (2)	0.668 (3)	0.601 (4)	0.026 (5)
C12	0.7926 (19)	0.769 (3)	0.507 (5)	0.021 (4)
H12A	0.686910	0.786221	0.489467	0.026*
H12B	0.894885	0.880918	0.577071	0.026*
C13	0.7993 (19)	0.688 (3)	0.343 (5)	0.024 (4)
H13	0.816513	0.772171	0.304841	0.028*
C2	0.788 (2)	0.197 (4)	0.813 (6)	0.029 (4)
H2A	0.907599	0.290114	0.880855	0.034*
H2B	0.779190	0.135875	0.704233	0.034*
C3	0.758 (2)	0.074 (3)	0.882 (5)	0.031 (5)
H3	0.844860	0.028019	0.876720	0.037*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0277 (12)	0.029 (2)	0.034 (6)	0.0130 (14)	0.014 (2)	0.015 (3)
O1	0.029 (3)	0.032 (5)	0.030 (7)	0.016 (3)	0.016 (4)	0.013 (5)
O2	0.041 (5)	0.033 (8)	0.035 (13)	0.018 (5)	0.023 (7)	0.016 (9)
O14	0.030 (4)	0.037 (5)	0.035 (7)	0.017 (3)	0.016 (4)	0.014 (5)
O4	0.043 (4)	0.037 (5)	0.039 (7)	0.014 (3)	0.014 (4)	0.024 (5)
O11	0.059 (4)	0.047 (5)	0.050 (7)	0.023 (3)	0.018 (4)	0.032 (5)
O1W	0.037 (5)	0.034 (8)	0.035 (13)	0.016 (5)	0.018 (7)	0.016 (8)
O13	0.036 (5)	0.048 (8)	0.042 (13)	0.023 (5)	0.019 (7)	0.019 (9)
O3	0.043 (5)	0.043 (8)	0.038 (13)	0.013 (5)	0.022 (7)	0.024 (9)
O12	0.053 (7)	0.058 (9)	0.053 (14)	0.026 (6)	0.024 (8)	0.026 (9)
O2W	0.063 (6)	0.058 (8)	0.063 (13)	0.031 (5)	0.023 (7)	0.030 (9)
N13	0.030 (5)	0.038 (8)	0.028 (13)	0.017 (5)	0.016 (7)	0.016 (9)
N3	0.042 (6)	0.036 (9)	0.036 (13)	0.014 (5)	0.020 (8)	0.021 (9)
C1	0.027 (4)	0.024 (5)	0.028 (7)	0.009 (3)	0.013 (4)	0.012 (5)
C4	0.021 (4)	0.019 (5)	0.019 (7)	0.006 (3)	0.006 (4)	0.012 (5)
C14	0.022 (4)	0.023 (5)	0.024 (7)	0.009 (3)	0.010 (4)	0.010 (5)
C11	0.027 (6)	0.026 (7)	0.026 (8)	0.013 (4)	0.009 (5)	0.013 (6)
C12	0.021 (5)	0.023 (5)	0.020 (7)	0.011 (4)	0.007 (4)	0.012 (5)
C13	0.024 (5)	0.025 (5)	0.023 (7)	0.009 (3)	0.012 (4)	0.012 (5)
C2	0.027 (4)	0.028 (5)	0.029 (7)	0.014 (3)	0.010 (4)	0.013 (5)
C3	0.031 (5)	0.031 (6)	0.032 (8)	0.017 (4)	0.013 (5)	0.015 (5)

Geometric parameters (Å, º)

Zn1—O1	1.93 (3)	N13—H13C	0.8900
Zn1—O14^i	1.978 (11)	N13—C13	1.52 (4)
Zn1—O4^ii	1.92 (2)	N3—H3A	0.8900
Zn1—O11	1.922 (8)	N3—H3B	0.8900
O1—C1	1.24 (3)	N3—H3C	0.8900
O2—C1	1.24 (3)	N3—C3	1.45 (4)
O14—C14	1.24 (4)	C1—C2	1.520 (17)
O4—C4	1.32 (2)	C4—C3	1.56 (3)
O11—C11	1.36 (2)	C14—C13	1.535 (18)
O1W—H1WA	0.8387	C11—C12	1.55 (3)
O1W—H1WB	0.8734	C12—H12A	0.9700
O13—C14	1.32 (5)	C12—H12B	0.9700
O3—C4	1.251 (19)	C12—C13	1.53 (3)
O12—C11	1.18 (3)	C13—H13	0.9800
O2W—H2WA	0.8413	C2—H2A	0.9700
O2W—H2WB	0.8471	C2—H2B	0.9700
N13—H13A	0.8900	C2—C3	1.53 (2)
N13—H13B	0.8900	C3—H3	0.9800
O1—Zn1—O14^i	119.1 (9)	O14—C14—O13	124.4 (15)
O4^ii—Zn1—O1	94.9 (9)	O14—C14—C13	117 (3)
O4^ii—Zn1—O14^i	102.6 (9)	O13—C14—C13	118 (3)
O4^ii—Zn1—O11	107.0 (8)	O11—C11—C12	107 (2)
O11—Zn1—O1	114.7 (8)	O12—C11—O11	131 (2)
O11—Zn1—O14^i	114.6 (5)	O12—C11—C12	122 (2)
C1—O1—Zn1	129.8 (19)	C11—C12—H12A	108.0
C14—O14—Zn1^i	111.2 (19)	C11—C12—H12B	108.0
C4—O4—Zn1^ii	122.8 (9)	H12A—C12—H12B	107.3
C11—O11—Zn1	123.3 (17)	C13—C12—C11	117.1 (19)
H1WA—O1W—H1WB	102.9	C13—C12—H12A	108.0
H2WA—O2W—H2WB	104.6	C13—C12—H12B	108.0
H13A—N13—H13B	109.5	N13—C13—C14	108 (2)
H13A—N13—H13C	109.5	N13—C13—C12	112.2 (17)
H13B—N13—H13C	109.5	N13—C13—H13	108.3
C13—N13—H13A	109.5	C14—C13—H13	108.3
C13—N13—H13B	108.0	C12—C13—C14	112 (3)
C13—N13—H13C	109.5	C12—C13—H13	108.3
H3A—N3—H3B	108.0	C1—C2—H2A	108.7
H3A—N3—H3C	106.0	C1—C2—H2B	108.7
H3B—N3—H3C	107.0	C1—C2—C3	114.2 (17)
C3—N3—H3A	112.0	H2A—C2—H2B	107.6
C3—N3—H3B	111.0	C3—C2—H2A	108.7
C3—N3—H3C	112.0	C3—C2—H2B	108.7
O1—C1—O2	120.5 (14)	N3—C3—C4	107.3 (19)
O1—C1—C2	120 (2)	N3—C3—C2	115 (3)
O2—C1—C2	120 (2)	N3—C3—H3	107.5
O4—C4—C3	112.9 (17)	C4—C3—H3	107.5
O3—C4—O4	130.2 (18)	C2—C3—C4	111 (2)
O3—C4—C3	116 (2)	C2—C3—H3	107.5
Zn1—O1—C1—C2	19 (5)	N13—C13—C14—O13	18 (3)
Zn1—O14^i—C14^i—C13^i	175.3 (18)	N3—C3—C4—O3	−33 (2)
Zn1—O4^ii—C4^ii—C3^ii	−170.8 (12)	C1—C2—C3—N3	−63 (4)
Zn1—O11—C11—C12	174.5 (8)	C1—C2—C3—C4	59 (4)
O2—C1—C2—C3	19 (5)	C11—C12—C13—N13	68.2 (15)
O12—C11—C12—C13	155 (2)	C11—C12—C13—C14	−52.9 (17)

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

(Zn-aspartate_dihydrate_0_70GPa)

Crystal data

C16H24N4O16Zn2·4(H2O)	Z = 1
Mr = 731.19	F(000) = 376
Triclinic, P1	Dx = 1.915 Mg m^−3
a = 8.687 (4) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.359 (3) Å	Cell parameters from 380 reflections
c = 9.7666 (19) Å	θ = 3.9–27.5°
α = 111.78 (3)°	µ = 2.00 mm^−1
β = 105.20 (3)°	T = 296 K
γ = 108.04 (4)°	Plate, colourless
V = 633.9 (4) Å^3	0.25 × 0.20 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.062
Radiation source: sealed x-ray tube	θmax = 27.5°, θmin = 3.9°
ω scan	h = −11→10
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −11→12
Tmin = 0.626, Tmax = 0.923	l = −7→7
2494 measured reflections	12 standard reflections every 84 reflections
470 independent reflections	intensity decay: none
380 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.040	H-atom parameters constrained
wR(F^2) = 0.102	w = 1/[σ^2(Fo^2) + (0.0703P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.10	(Δ/σ)max < 0.001
470 reflections	Δρmax = 0.20 e Å^−3
198 parameters	Δρmin = −0.17 e Å^−3
131 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 0.70 (2) GPa (700000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7121 (2)	0.3223 (4)	0.5440 (6)	0.029 (2)
O1	0.6421 (18)	0.341 (3)	0.719 (5)	0.029 (3)
O2	0.5714 (15)	0.270 (2)	0.887 (4)	0.034 (5)
O14	1.1015 (16)	0.753 (3)	0.469 (4)	0.034 (3)
O4	0.5021 (18)	−0.120 (2)	0.622 (4)	0.039 (4)
O11	0.7234 (15)	0.499 (2)	0.488 (4)	0.050 (3)
O1W	0.2287 (16)	0.025 (3)	0.768 (4)	0.034 (5)
H1WA	0.339886	0.079936	0.819928	0.052*
H1WB	0.210615	−0.080955	0.717181	0.052*
O13	0.9266 (17)	0.497 (3)	0.235 (4)	0.040 (5)
O3	0.5108 (14)	−0.162 (2)	0.844 (3)	0.040 (5)
O12	0.843 (2)	0.736 (3)	0.744 (4)	0.053 (7)
O2W	0.2233 (17)	0.316 (3)	0.999 (4)	0.060 (5)
H2WA	0.240366	0.229198	0.953232	0.090*
H2WB	0.178022	0.294565	1.061132	0.090*
N13	0.6285 (19)	0.527 (3)	0.214 (5)	0.030 (5)
H13A	0.636167	0.482799	0.121891	0.035*
H13B	0.539355	0.554456	0.201408	0.035*
H13C	0.608602	0.450977	0.249310	0.035*
N3	0.782 (2)	0.150 (3)	1.050 (4)	0.036 (6)
H3A	0.711687	0.201226	1.064078	0.038*
H3B	0.894515	0.228842	1.117093	0.038*
H3C	0.756227	0.072026	1.082374	0.038*
C1	0.657 (2)	0.272 (4)	0.804 (6)	0.026 (3)
C4	0.5678 (18)	−0.083 (2)	0.776 (4)	0.020 (4)
C14	0.954 (2)	0.641 (4)	0.355 (6)	0.023 (4)
C11	0.791 (2)	0.668 (3)	0.601 (4)	0.026 (5)
C12	0.7927 (19)	0.769 (3)	0.508 (5)	0.021 (4)
H12A	0.686522	0.786685	0.490410	0.025*
H12B	0.895539	0.881955	0.577242	0.025*
C13	0.7995 (19)	0.689 (3)	0.344 (5)	0.023 (4)
H13	0.817634	0.773778	0.306041	0.028*
C2	0.788 (2)	0.197 (4)	0.813 (6)	0.028 (3)
H2A	0.908190	0.290835	0.880102	0.034*
H2B	0.779127	0.135154	0.704223	0.034*
C3	0.758 (2)	0.074 (3)	0.882 (5)	0.030 (5)
H3	0.845445	0.028127	0.877040	0.036*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0273 (12)	0.028 (2)	0.033 (6)	0.0126 (14)	0.014 (2)	0.014 (3)
O1	0.028 (3)	0.031 (5)	0.029 (7)	0.015 (3)	0.016 (4)	0.012 (5)
O2	0.040 (5)	0.032 (8)	0.034 (13)	0.018 (5)	0.023 (7)	0.015 (9)
O14	0.030 (4)	0.036 (5)	0.034 (7)	0.017 (3)	0.016 (4)	0.013 (5)
O4	0.042 (4)	0.036 (5)	0.038 (7)	0.014 (3)	0.014 (4)	0.023 (5)
O11	0.057 (4)	0.046 (5)	0.049 (7)	0.022 (3)	0.017 (4)	0.031 (5)
O1W	0.037 (5)	0.033 (8)	0.034 (13)	0.015 (5)	0.017 (7)	0.016 (8)
O13	0.035 (5)	0.047 (8)	0.041 (13)	0.022 (5)	0.018 (7)	0.019 (9)
O3	0.042 (5)	0.042 (8)	0.037 (13)	0.012 (4)	0.021 (7)	0.024 (8)
O12	0.052 (7)	0.057 (9)	0.051 (14)	0.026 (5)	0.023 (8)	0.025 (9)
O2W	0.062 (6)	0.056 (8)	0.062 (13)	0.030 (5)	0.022 (7)	0.030 (9)
N13	0.029 (5)	0.037 (8)	0.027 (13)	0.016 (5)	0.015 (7)	0.016 (9)
N3	0.041 (6)	0.035 (9)	0.035 (13)	0.014 (5)	0.020 (8)	0.021 (9)
C1	0.026 (4)	0.023 (5)	0.027 (7)	0.009 (3)	0.012 (4)	0.012 (5)
C4	0.020 (4)	0.018 (5)	0.019 (7)	0.005 (3)	0.006 (4)	0.012 (5)
C14	0.021 (4)	0.023 (5)	0.023 (7)	0.009 (3)	0.010 (4)	0.010 (5)
C11	0.026 (6)	0.025 (7)	0.026 (8)	0.013 (4)	0.009 (5)	0.013 (6)
C12	0.021 (5)	0.023 (5)	0.020 (7)	0.011 (4)	0.007 (4)	0.012 (5)
C13	0.023 (5)	0.025 (5)	0.022 (7)	0.009 (3)	0.012 (4)	0.012 (5)
C2	0.027 (4)	0.027 (5)	0.028 (7)	0.014 (3)	0.010 (4)	0.012 (5)
C3	0.030 (5)	0.030 (6)	0.031 (8)	0.017 (4)	0.012 (5)	0.014 (5)

Geometric parameters (Å, º)

Zn1—O1	1.93 (3)	N13—H13C	0.8900
Zn1—O14^i	1.968 (11)	N13—C13	1.52 (4)
Zn1—O4^ii	1.91 (2)	N3—H3A	0.8900
Zn1—O11	1.911 (8)	N3—H3B	0.8900
O1—C1	1.23 (3)	N3—H3C	0.8900
O2—C1	1.24 (3)	N3—C3	1.45 (4)
O14—C14	1.24 (4)	C1—C2	1.512 (2)
O4—C4	1.32 (2)	C4—C3	1.56 (3)
O11—C11	1.36 (2)	C14—C13	1.529 (2)
O1W—H1WA	0.8347	C11—C12	1.54 (3)
O1W—H1WB	0.8685	C12—H12A	0.9700
O13—C14	1.32 (5)	C12—H12B	0.9700
O3—C4	1.244 (19)	C12—C13	1.520 (3)
O12—C11	1.18 (3)	C13—H13	0.9800
O2W—H2WA	0.8502	C2—H2A	0.9700
O2W—H2WB	0.8499	C2—H2B	0.9700
N13—H13A	0.8700	C2—C3	1.530 (2)
N13—H13B	0.8900	C3—H3	0.9800
O1—Zn1—O14^i	119.0 (9)	O14—C14—O13	124.6 (15)
O4^ii—Zn1—O1	95.4 (8)	O14—C14—C13	116 (3)
O4^ii—Zn1—O14^i	102.5 (9)	O13—C14—C13	118 (3)
O4^ii—Zn1—O11	106.5 (8)	O11—C11—C12	106 (2)
O11—Zn1—O1	114.8 (8)	O12—C11—O11	131 (2)
O11—Zn1—O14^i	114.7 (5)	O12—C11—C12	122 (2)
C1—O1—Zn1	129.8 (19)	C11—C12—H12A	108.0
C14—O14—Zn1^i	111.0 (19)	C11—C12—H12B	108.0
C4—O4—Zn1^ii	123.1 (9)	H12A—C12—H12B	107.2
C11—O11—Zn1	122.7 (17)	C13—C12—C11	117.3 (19)
H1WA—O1W—H1WB	102.9	C13—C12—H12A	108.0
H2WA—O2W—H2WB	104.4	C13—C12—H12B	108.0
H13A—N13—H13B	109.5	N13—C13—C14	107 (2)
H13A—N13—H13C	109.5	N13—C13—C12	112.8 (17)
H13B—N13—H13C	109.5	N13—C13—H13	108.2
C13—N13—H13A	111.0	C14—C13—H13	108.2
C13—N13—H13B	108.0	C12—C13—C14	112 (3)
C13—N13—H13C	108.0	C12—C13—H13	108.2
H3A—N3—H3B	108.0	C1—C2—H2A	108.7
H3A—N3—H3C	107.0	C1—C2—H2B	108.7
H3B—N3—H3C	107.0	C1—C2—C3	114.2 (17)
C3—N3—H3A	111.0	H2A—C2—H2B	107.6
C3—N3—H3B	111.0	C3—C2—H2A	108.7
C3—N3—H3C	112.0	C3—C2—H2B	108.7
O1—C1—O2	120.6 (14)	N3—C3—C4	107.9 (19)
O1—C1—C2	120 (2)	N3—C3—C2	116 (3)
O2—C1—C2	120 (2)	N3—C3—H3	107.4
O4—C4—C3	113.4 (17)	C4—C3—H3	107.4
O3—C4—O4	130.5 (18)	C2—C3—C4	111 (2)
O3—C4—C3	116 (2)	C2—C3—H3	107.4
O2—C1—C2—C3	19 (5)	C1—C2—C3—N3	−63 (4)
O12—C11—C12—C13	155 (2)	C1—C2—C3—C4	60 (4)
N13—C13—C14—O13	18 (3)	C11—C12—C13—N13	68.5 (15)
N3—C3—C4—O3	−33 (2)	C11—C12—C13—C14	−52.8 (17)

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

(Zn-aspartate_dihydrate_1_02GPa)

Crystal data

C16H24N4O16Zn2·4(H2O)	Z = 1
Mr = 731.19	F(000) = 376
Triclinic, P1	Dx = 1.932 Mg m^−3
a = 8.668 (4) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.308 (4) Å	Cell parameters from 325 reflections
c = 9.738 (3) Å	θ = 3.9–27.1°
α = 111.52 (3)°	µ = 2.01 mm^−1
β = 105.23 (3)°	T = 296 K
γ = 108.10 (4)°	Plate, colourless
V = 628.5 (5) Å^3	0.25 × 0.20 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.107
Radiation source: sealed x-ray tube	θmax = 27.1°, θmin = 3.9°
ω scan	h = −4→4
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −9→9
Tmin = 0.623, Tmax = 0.904	l = −12→12
2540 measured reflections	12 standard reflections every 84 reflections
461 independent reflections	intensity decay: none
325 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.053	H-atom parameters constrained
wR(F^2) = 0.139	w = 1/[σ^2(Fo^2) + (0.0402P)^2 + 6.9565P] where P = (Fo^2 + 2Fc^2)/3
S = 1.11	(Δ/σ)max < 0.001
461 reflections	Δρmax = 0.26 e Å^−3
199 parameters	Δρmin = −0.39 e Å^−3
139 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 1.02 (2) GPa (1020000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7053 (17)	0.3217 (6)	0.5392 (3)	0.041 (3)
O1	0.638 (6)	0.342 (2)	0.7190 (16)	0.048 (5)
O2	0.581 (4)	0.276 (2)	0.9004 (15)	0.046 (7)
O14	1.095 (7)	0.757 (3)	0.466 (2)	0.037 (7)
O4	0.504 (5)	−0.114 (2)	0.6331 (14)	0.039 (5)
O11	0.711 (7)	0.508 (3)	0.4925 (14)	0.032 (5)
O1W	0.244 (6)	0.027 (2)	0.7768 (16)	0.040 (7)
H1WA	0.349293	0.119518	0.832847	0.060*
H1WB	0.243468	−0.025443	0.683768	0.060*
O13	0.949 (6)	0.501 (2)	0.2512 (17)	0.052 (8)
O3	0.510 (5)	−0.164 (2)	0.8426 (14)	0.038 (7)
O12	0.838 (6)	0.732 (2)	0.7369 (15)	0.043 (7)
O2W	0.226 (6)	0.320 (3)	1.0042 (19)	0.053 (8)
H2WA	0.232398	0.224308	0.972901	0.080*
H2WB	0.229006	0.346346	1.098466	0.080*
N13	0.634 (9)	0.539 (4)	0.213 (2)	0.045 (8)
H13A	0.636167	0.482799	0.121891	0.035*
H13B	0.539355	0.554456	0.201408	0.035*
H13C	0.608602	0.450977	0.249310	0.035*
N3	0.780 (7)	0.155 (3)	1.0551 (19)	0.041 (8)
H3A	0.711687	0.201226	1.064078	0.038*
H3B	0.894515	0.228842	1.117093	0.038*
H3C	0.756227	0.072026	1.082374	0.038*
C4	0.588 (7)	−0.084 (2)	0.780 (2)	0.034 (6)
C13	0.797 (6)	0.690 (3)	0.337 (2)	0.032 (9)
H13	0.818294	0.774433	0.298743	0.038*
C11	0.775 (9)	0.668 (3)	0.590 (2)	0.040 (7)
C12	0.792 (5)	0.777 (2)	0.5024 (18)	0.031 (6)
H12A	0.691699	0.804107	0.486358	0.038*
H12B	0.900949	0.885359	0.573198	0.038*
C14	0.951 (5)	0.644 (3)	0.355 (3)	0.040 (10)
C3	0.767 (5)	0.073 (2)	0.8880 (18)	0.035 (6)
H3	0.860409	0.034959	0.891169	0.042*
C2	0.802 (7)	0.208 (3)	0.827 (3)	0.041 (9)
H2A	0.920053	0.305139	0.901399	0.049*
H2B	0.800767	0.155444	0.720483	0.049*
C1	0.661 (5)	0.275 (3)	0.817 (3)	0.026 (8)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.048 (6)	0.039 (3)	0.0386 (16)	0.022 (3)	0.013 (3)	0.0245 (15)
O1	0.050 (8)	0.049 (6)	0.047 (5)	0.022 (4)	0.019 (5)	0.026 (5)
O2	0.050 (13)	0.048 (8)	0.045 (6)	0.019 (6)	0.021 (9)	0.029 (6)
O14	0.036 (9)	0.035 (8)	0.042 (8)	0.012 (4)	0.018 (6)	0.021 (6)
O4	0.041 (8)	0.042 (6)	0.035 (5)	0.019 (4)	0.017 (5)	0.020 (5)
O11	0.031 (7)	0.032 (5)	0.034 (5)	0.012 (4)	0.015 (5)	0.017 (4)
O1W	0.040 (13)	0.039 (8)	0.039 (6)	0.020 (7)	0.017 (9)	0.016 (6)
O13	0.051 (13)	0.054 (9)	0.050 (7)	0.024 (7)	0.025 (10)	0.022 (6)
O3	0.042 (12)	0.034 (7)	0.039 (6)	0.021 (6)	0.013 (9)	0.017 (5)
O12	0.044 (13)	0.049 (8)	0.035 (6)	0.023 (7)	0.016 (9)	0.018 (6)
O2W	0.056 (14)	0.057 (9)	0.049 (7)	0.027 (7)	0.025 (9)	0.025 (7)
N13	0.047 (14)	0.046 (10)	0.045 (8)	0.022 (7)	0.017 (10)	0.023 (7)
N3	0.041 (13)	0.038 (9)	0.043 (7)	0.020 (7)	0.010 (9)	0.022 (7)
C4	0.034 (9)	0.033 (7)	0.035 (7)	0.015 (4)	0.013 (6)	0.018 (6)
C13	0.032 (10)	0.031 (9)	0.033 (9)	0.013 (5)	0.013 (6)	0.017 (6)
C11	0.040 (9)	0.041 (8)	0.039 (7)	0.019 (4)	0.016 (6)	0.019 (6)
C12	0.032 (8)	0.031 (7)	0.032 (6)	0.014 (4)	0.013 (6)	0.017 (5)
C14	0.040 (12)	0.039 (11)	0.040 (10)	0.017 (5)	0.016 (7)	0.022 (7)
C3	0.035 (9)	0.036 (7)	0.034 (6)	0.017 (4)	0.013 (6)	0.018 (5)
C2	0.041 (11)	0.040 (10)	0.042 (10)	0.018 (5)	0.017 (7)	0.021 (7)
C1	0.026 (10)	0.024 (8)	0.029 (8)	0.012 (5)	0.010 (6)	0.013 (6)

Geometric parameters (Å, º)

Zn1—O1	1.95 (3)	N13—H13C	0.9900
Zn1—O14^i	2.08 (6)	N13—C13	1.43 (4)
Zn1—O4^ii	1.920 (19)	N3—H3A	0.8400
Zn1—O11	1.93 (4)	N3—H3B	0.8900
O1—C1	1.33 (4)	N3—H3C	0.8900
O2—C1	1.20 (3)	N3—C3	1.48 (3)
O14—C14	1.21 (3)	C4—C3	1.50 (3)
O4—C4	1.30 (4)	C13—H13	0.9800
O11—C11	1.26 (4)	C13—C12	1.53 (2)
O1W—H1WA	0.8798	C13—C14	1.51 (3)
O1W—H1WB	0.8543	C11—C12	1.54 (3)
O13—C14	1.34 (3)	C12—H12A	0.9700
O3—C4	1.27 (2)	C12—H12B	0.9700
O12—C11	1.21 (2)	C3—H3	0.9800
O2W—H2WA	0.8500	C3—C2	1.56 (3)
O2W—H2WB	0.8499	C2—H2A	0.9700
N13—H13A	0.8600	C2—H2B	0.9700
N13—H13B	0.8600	C2—C1	1.53 (6)
O1—Zn1—O14^i	116.3 (18)	C12—C13—H13	107.2
O4^ii—Zn1—O1	98.5 (10)	C14—C13—H13	107.2
O4^ii—Zn1—O14^i	100.9 (16)	C14—C13—C12	110.8 (17)
O4^ii—Zn1—O11	107.7 (16)	O11—C11—C12	112.5 (13)
O11—Zn1—O1	111 (2)	O12—C11—O11	124 (3)
O11—Zn1—O14^i	119 (2)	O12—C11—C12	122 (2)
C1—O1—Zn1	131 (4)	C13—C12—C11	115 (2)
C14—O14—Zn1^i	111 (3)	C13—C12—H12A	108.6
C4—O4—Zn1^ii	126.2 (10)	C13—C12—H12B	108.6
C11—O11—Zn1	129 (2)	C11—C12—H12A	108.6
H1WA—O1W—H1WB	103.9	C11—C12—H12B	108.6
H2WA—O2W—H2WB	104.5	H12A—C12—H12B	107.6
H13A—N13—H13B	113.0	O14—C14—O13	117 (4)
H13A—N13—H13C	102.0	O14—C14—C13	116 (4)
H13B—N13—H13C	101.0	O13—C14—C13	126 (3)
C13—N13—H13A	116.0	N3—C3—C4	109 (2)
C13—N13—H13B	114.0	N3—C3—H3	108.0
C13—N13—H13C	109.5	N3—C3—C2	110 (2)
H3A—N3—H3B	113.0	C4—C3—H3	108.0
H3A—N3—H3C	111.0	C4—C3—C2	113.7 (19)
H3B—N3—H3C	107.0	C2—C3—H3	108.0
C3—N3—H3A	114.0	C3—C2—H2A	109.3
C3—N3—H3B	105.0	C3—C2—H2B	109.3
C3—N3—H3C	106.0	H2A—C2—H2B	107.9
O4—C4—C3	117.8 (13)	C1—C2—C3	112 (3)
O3—C4—O4	122 (3)	C1—C2—H2A	109.3
O3—C4—C3	119.4 (18)	C1—C2—H2B	109.3
N13—C13—H13	107.2	O1—C1—C2	117 (3)
N13—C13—C12	115 (3)	O2—C1—O1	121 (4)
N13—C13—C14	109 (4)	O2—C1—C2	122 (3)
Zn1—O1—C1—C2	18 (3)	N13—C13—C14—O13	14 (3)
Zn1—O14^i—C14^i—C13^i	175.6 (15)	N3—C3—C4—O3	−27 (5)
Zn1—O4^ii—C4^ii—C3^ii	−169 (3)	C11—C12—C13—N13	66 (5)
Zn1—O11—C11—C12	167 (4)	C11—C12—C13—C14	−58 (4)
O2—C1—C2—C3	26 (3)	C1—C2—C3—N3	−63 (4)
O12—C11—C12—C13	150 (6)	C1—C2—C3—C4	60 (3)

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

(Zn-aspartate_dihydrate_1_54GPa)

Crystal data

C16H24N4O16Zn2·4(H2O)	Z = 1
Mr = 731.19	F(000) = 376
Triclinic, P1	Dx = 1.971 Mg m^−3
a = 8.594 (4) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.235 (3) Å	Cell parameters from 314 reflections
c = 9.6951 (16) Å	θ = 3.9–26.7°
α = 111.39 (2)°	µ = 2.05 mm^−1
β = 104.94 (2)°	T = 296 K
γ = 108.42 (3)°	Plate, colourless
V = 616.2 (4) Å^3	0.25 × 0.20 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.115
Radiation source: sealed x-ray tube	θmax = 26.7°, θmin = 3.9°
ω scan	h = −4→4
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −9→9
Tmin = 0.617, Tmax = 0.902	l = −12→12
2559 measured reflections	12 standard reflections every 84 reflections
458 independent reflections	intensity decay: none
314 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.049	H-atom parameters constrained
wR(F^2) = 0.142	w = 1/[σ^2(Fo^2) + (0.0615P)^2 + 3.7775P] where P = (Fo^2 + 2Fc^2)/3
S = 1.12	(Δ/σ)max < 0.001
458 reflections	Δρmax = 0.25 e Å^−3
198 parameters	Δρmin = −0.26 e Å^−3
136 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 1.54 (2) GPa (1540000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.7017 (16)	0.3212 (6)	0.5364 (3)	0.036 (3)
O1	0.636 (5)	0.342 (2)	0.7185 (14)	0.040 (5)
O2	0.580 (4)	0.2784 (18)	0.9021 (13)	0.036 (7)
O14	1.087 (6)	0.760 (3)	0.4713 (18)	0.038 (7)
O4	0.504 (5)	−0.1102 (19)	0.6355 (13)	0.036 (5)
O11	0.711 (6)	0.508 (2)	0.4911 (13)	0.032 (5)
O1W	0.245 (6)	0.029 (2)	0.7768 (14)	0.040 (7)
H1WA	0.345785	0.121739	0.812882	0.060*
H1WB	0.251170	−0.051045	0.702144	0.060*
O13	0.945 (5)	0.506 (3)	0.2532 (18)	0.055 (8)
O3	0.514 (5)	−0.1650 (18)	0.8437 (13)	0.038 (7)
O12	0.834 (5)	0.734 (2)	0.7368 (14)	0.040 (7)
O2W	0.224 (6)	0.321 (2)	1.0072 (15)	0.043 (8)
H2WA	0.242281	0.236081	0.963754	0.065*
H2WB	0.218624	0.329127	1.089515	0.065*
N13	0.641 (8)	0.537 (3)	0.2115 (19)	0.033 (7)
H13A	0.636167	0.482799	0.121891	0.035*
H13B	0.539355	0.554456	0.201408	0.035*
H13C	0.608602	0.450977	0.249310	0.035*
N3	0.790 (6)	0.156 (3)	1.0600 (14)	0.038 (7)
H3A	0.711687	0.201226	1.064078	0.038*
H3B	0.894515	0.228842	1.117093	0.038*
H3C	0.756227	0.072026	1.082374	0.038*
C2	0.805 (5)	0.213 (3)	0.833 (3)	0.040 (9)
H2A	0.922178	0.312603	0.910182	0.048*
H2B	0.810741	0.162296	0.728518	0.048*
C4	0.601 (11)	−0.085 (4)	0.7873 (18)	0.034 (6)
C14	0.945 (4)	0.646 (3)	0.353 (2)	0.030 (9)
C11	0.765 (8)	0.675 (3)	0.590 (2)	0.035 (6)
C12	0.787 (5)	0.780 (2)	0.5025 (17)	0.027 (6)
H12A	0.897622	0.888609	0.574246	0.033*
H12B	0.687663	0.810572	0.486762	0.033*
C13	0.793 (6)	0.697 (3)	0.337 (2)	0.035 (9)
H13	0.813820	0.781970	0.297877	0.042*
C1	0.662 (4)	0.277 (3)	0.815 (2)	0.022 (7)
C3	0.772 (5)	0.078 (2)	0.8915 (18)	0.039 (6)
H3	0.868910	0.043949	0.893936	0.047*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.044 (6)	0.035 (2)	0.0338 (14)	0.020 (3)	0.015 (3)	0.0204 (13)
O1	0.043 (7)	0.042 (6)	0.037 (5)	0.022 (4)	0.016 (5)	0.019 (4)
O2	0.037 (12)	0.039 (7)	0.032 (5)	0.017 (6)	0.015 (8)	0.018 (5)
O14	0.037 (9)	0.038 (8)	0.039 (7)	0.015 (4)	0.020 (6)	0.018 (5)
O4	0.037 (7)	0.036 (6)	0.036 (5)	0.018 (4)	0.015 (5)	0.017 (4)
O11	0.031 (7)	0.031 (5)	0.033 (4)	0.015 (4)	0.011 (5)	0.017 (4)
O1W	0.037 (13)	0.041 (8)	0.040 (6)	0.015 (7)	0.013 (9)	0.021 (6)
O13	0.052 (13)	0.053 (8)	0.058 (7)	0.020 (7)	0.031 (9)	0.025 (6)
O3	0.040 (12)	0.036 (7)	0.037 (5)	0.014 (6)	0.017 (8)	0.020 (5)
O12	0.042 (13)	0.048 (8)	0.031 (5)	0.024 (7)	0.017 (8)	0.014 (6)
O2W	0.040 (13)	0.046 (9)	0.041 (7)	0.023 (7)	0.019 (9)	0.014 (6)
N13	0.031 (13)	0.032 (8)	0.033 (7)	0.019 (7)	0.009 (10)	0.012 (6)
N3	0.041 (13)	0.037 (8)	0.036 (7)	0.020 (7)	0.007 (9)	0.021 (6)
C2	0.041 (11)	0.040 (10)	0.041 (9)	0.016 (5)	0.017 (7)	0.023 (6)
C4	0.035 (9)	0.034 (7)	0.036 (6)	0.014 (4)	0.016 (6)	0.019 (5)
C14	0.031 (11)	0.030 (10)	0.030 (9)	0.012 (5)	0.013 (6)	0.019 (7)
C11	0.034 (8)	0.034 (7)	0.034 (6)	0.017 (4)	0.013 (6)	0.014 (5)
C12	0.027 (8)	0.026 (6)	0.030 (6)	0.010 (4)	0.015 (6)	0.015 (5)
C13	0.035 (11)	0.033 (10)	0.036 (9)	0.017 (5)	0.013 (6)	0.017 (6)
C1	0.023 (9)	0.021 (8)	0.024 (7)	0.010 (5)	0.009 (6)	0.012 (6)
C3	0.039 (9)	0.038 (7)	0.041 (7)	0.017 (4)	0.017 (6)	0.020 (6)

Geometric parameters (Å, º)

Zn1—O1	1.95 (2)	N13—H13C	0.9800
Zn1—O14^i	2.18 (6)	N13—C13	1.42 (3)
Zn1—O4^ii	1.907 (16)	N3—H3A	0.8900
Zn1—O11	1.91 (4)	N3—H3B	0.8100
O1—C1	1.29 (4)	N3—H3C	0.8600
O2—C1	1.23 (2)	N3—C3	1.47 (3)
O14—C14	1.22 (2)	C2—H2A	0.9700
O4—C4	1.38 (5)	C2—H2B	0.9700
O11—C11	1.33 (4)	C2—C1	1.52 (3)
O1W—H1WA	0.8702	C2—C3	1.53 (2)
O1W—H1WB	0.8516	C4—C3	1.47 (4)
O13—C14	1.30 (3)	C14—C13	1.52 (4)
O3—C4	1.25 (3)	C11—C12	1.50 (3)
O12—C11	1.22 (2)	C12—H12A	0.9700
O2W—H2WA	0.8293	C12—H12B	0.9700
O2W—H2WB	0.7900	C12—C13	1.53 (2)
N13—H13A	0.8100	C13—H13	0.9800
N13—H13B	0.9200	C3—H3	0.9800
O1—Zn1—O14^i	116.4 (16)	O4—C4—C3	115.9 (15)
O4^ii—Zn1—O1	99.6 (10)	O3—C4—O4	117 (5)
O4^ii—Zn1—O14^i	99.6 (15)	O3—C4—C3	122.8 (15)
O4^ii—Zn1—O11	109.1 (15)	O14—C14—O13	119 (4)
O11—Zn1—O1	111.7 (19)	O14—C14—C13	113 (4)
O11—Zn1—O14^i	117.7 (19)	O13—C14—C13	128 (3)
C1—O1—Zn1	131 (4)	O11—C11—C12	111.8 (13)
C14—O14—Zn1^i	108 (3)	O12—C11—O11	119 (3)
C4—O4—Zn1^ii	125.2 (10)	O12—C11—C12	125.5 (15)
C11—O11—Zn1	131.3 (14)	C11—C12—H12A	107.9
H1WA—O1W—H1WB	104.0	C11—C12—H12B	107.9
H2WA—O2W—H2WB	109.0	C11—C12—C13	118 (2)
H13A—N13—H13B	109.5	H12A—C12—H12B	107.2
H13A—N13—H13C	105.0	C13—C12—H12A	107.9
H13B—N13—H13C	96.0	C13—C12—H12B	107.9
C13—N13—H13A	123.0	N13—C13—C14	102 (4)
C13—N13—H13B	107.0	N13—C13—C12	118 (3)
C13—N13—H13C	112.0	N13—C13—H13	108.8
H3A—N3—H3B	113.0	C14—C13—C12	110.6 (18)
H3A—N3—H3C	107.0	C14—C13—H13	108.8
H3B—N3—H3C	114.0	C12—C13—H13	108.8
C3—N3—H3A	108.0	O1—C1—C2	121 (3)
C3—N3—H3B	107.0	O2—C1—O1	120 (4)
C3—N3—H3C	107.0	O2—C1—C2	119 (3)
H2A—C2—H2B	107.7	N3—C3—C2	111.0 (18)
C1—C2—H2A	108.8	N3—C3—C4	110 (2)
C1—C2—H2B	108.8	N3—C3—H3	106.3
C1—C2—C3	113.9 (17)	C2—C3—H3	106.3
C3—C2—H2A	108.8	C4—C3—C2	116 (2)
C3—C2—H2B	108.8	C4—C3—H3	106.3
Zn1—O1—C1—C2	20 (3)	N13—C13—C14—O13	14 (3)
Zn1—O14^i—C14^i—C13^i	174.2 (14)	N3—C3—C4—O3	−18 (10)
Zn1—O4^ii—C4^ii—C3^ii	−170 (4)	C11—C12—C13—N13	59 (5)
Zn1—O11—C11—C12	167 (4)	C11—C12—C13—C14	−58 (4)
O2—C1—C2—C3	29 (3)	C1—C2—C3—N3	−67 (4)
O12—C11—C12—C13	145 (5)	C1—C2—C3—C4	59 (5)

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

(Zn-aspartate_dihydrate_2_53GPa)

Crystal data

C16H24N4O16Zn2·4(H2O)	Z = 1
Mr = 731.19	F(000) = 376
Triclinic, P1	Dx = 2.032 Mg m^−3
a = 8.484 (3) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.110 (3) Å	Cell parameters from 319 reflections
c = 9.6213 (14) Å	θ = 4.0–27.1°
α = 110.91 (2)°	µ = 2.12 mm^−1
β = 104.75 (2)°	T = 296 K
γ = 108.76 (3)°	Plate, colourless
V = 597.6 (3) Å^3	0.25 × 0.20 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.106
Radiation source: sealed x-ray tube	θmax = 27.1°, θmin = 4.0°
ω scan	h = −4→4
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −9→8
Tmin = 0.608, Tmax = 0.900	l = −12→12
2469 measured reflections	12 standard reflections every 84 reflections
444 independent reflections	intensity decay: none
319 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.051	H-atom parameters constrained
wR(F^2) = 0.141	w = 1/[σ^2(Fo^2) + (0.074P)^2 + 4.5648P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max < 0.001
444 reflections	Δρmax = 0.29 e Å^−3
198 parameters	Δρmin = −0.27 e Å^−3
134 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 2.53 (2) GPa (2530000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.6989 (18)	0.3200 (8)	0.5311 (3)	0.030 (3)
O1	0.644 (5)	0.338 (2)	0.7171 (14)	0.034 (5)
O2	0.586 (4)	0.281 (2)	0.9072 (13)	0.032 (7)
O14	1.108 (7)	0.761 (4)	0.480 (2)	0.043 (9)
O4	0.525 (5)	−0.109 (2)	0.6398 (14)	0.029 (5)
O11	0.699 (7)	0.511 (3)	0.4876 (14)	0.032 (5)
O1W	0.237 (6)	0.033 (2)	0.7766 (14)	0.029 (7)
H1WA	0.348749	0.108103	0.811188	0.044*
H1WB	0.205179	−0.031224	0.675390	0.044*
O13	0.953 (5)	0.505 (3)	0.2591 (18)	0.048 (8)
O3	0.519 (5)	−0.167 (2)	0.8465 (13)	0.033 (7)
O12	0.834 (5)	0.736 (2)	0.7340 (13)	0.031 (7)
O2W	0.237 (5)	0.319 (3)	1.0099 (15)	0.039 (7)
H2WA	0.181869	0.210974	0.956312	0.058*
H2WB	0.208858	0.346307	1.089051	0.058*
N13	0.628 (2)	0.526 (2)	0.215 (17)	0.030 (7)
H13A	0.636167	0.482799	0.121891	0.035*
H13B	0.539355	0.554456	0.201408	0.035*
H13C	0.608602	0.450977	0.249310	0.035*
N3	0.790 (6)	0.156 (3)	1.0600 (14)	0.032 (8)
H3A	0.711687	0.201226	1.064078	0.038*
H3B	0.894515	0.228842	1.117093	0.038*
H3C	0.756227	0.072026	1.082374	0.038*
C2	0.815 (5)	0.216 (3)	0.831 (3)	0.033 (9)
H2A	0.935600	0.315171	0.903852	0.040*
H2B	0.813846	0.162494	0.723152	0.040*
C4	0.599 (7)	−0.083 (3)	0.787 (2)	0.029 (6)
C14	0.954 (6)	0.647 (3)	0.359 (3)	0.024 (9)
C11	0.775 (8)	0.672 (4)	0.586 (2)	0.029 (6)
C12	0.805 (7)	0.778 (3)	0.4998 (18)	0.028 (6)
H12A	0.712606	0.819791	0.491530	0.033*
H12B	0.922565	0.881743	0.570380	0.033*
C13	0.802 (6)	0.703 (4)	0.342 (3)	0.026 (9)
H13	0.829338	0.793724	0.307141	0.031*
C1	0.672 (5)	0.283 (3)	0.821 (3)	0.026 (8)
C3	0.781 (5)	0.078 (3)	0.8938 (18)	0.031 (6)
H3	0.874335	0.037145	0.888835	0.038*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.028 (5)	0.034 (2)	0.0264 (13)	0.013 (3)	0.002 (3)	0.0206 (14)
O1	0.036 (7)	0.040 (6)	0.028 (5)	0.018 (4)	0.013 (5)	0.018 (4)
O2	0.030 (12)	0.036 (8)	0.030 (6)	0.014 (6)	0.008 (8)	0.020 (6)
O14	0.042 (10)	0.044 (9)	0.041 (9)	0.023 (5)	0.019 (6)	0.016 (6)
O4	0.031 (7)	0.028 (5)	0.029 (5)	0.015 (4)	0.010 (5)	0.014 (4)
O11	0.034 (7)	0.033 (6)	0.030 (5)	0.016 (4)	0.011 (5)	0.017 (4)
O1W	0.032 (12)	0.033 (8)	0.025 (6)	0.018 (6)	0.013 (8)	0.012 (6)
O13	0.043 (13)	0.045 (9)	0.052 (7)	0.018 (7)	0.018 (9)	0.022 (7)
O3	0.031 (12)	0.031 (7)	0.035 (6)	0.011 (6)	0.006 (8)	0.021 (5)
O12	0.035 (12)	0.038 (8)	0.021 (5)	0.025 (7)	0.006 (8)	0.013 (6)
O2W	0.041 (13)	0.045 (8)	0.032 (6)	0.021 (6)	0.014 (9)	0.020 (6)
N13	0.031 (13)	0.032 (9)	0.026 (7)	0.018 (7)	0.006 (10)	0.015 (6)
N3	0.031 (13)	0.029 (9)	0.033 (7)	0.015 (7)	0.003 (9)	0.018 (7)
C2	0.034 (10)	0.034 (9)	0.034 (9)	0.014 (5)	0.014 (6)	0.019 (6)
C4	0.030 (8)	0.029 (7)	0.029 (6)	0.012 (4)	0.012 (6)	0.017 (5)
C14	0.024 (11)	0.024 (10)	0.025 (9)	0.010 (5)	0.010 (7)	0.013 (7)
C11	0.030 (8)	0.028 (7)	0.031 (6)	0.013 (4)	0.013 (6)	0.014 (5)
C12	0.027 (8)	0.028 (7)	0.028 (6)	0.014 (4)	0.011 (6)	0.012 (5)
C13	0.026 (11)	0.028 (10)	0.024 (9)	0.012 (5)	0.011 (6)	0.013 (6)
C1	0.027 (10)	0.026 (9)	0.027 (8)	0.012 (5)	0.011 (6)	0.013 (6)
C3	0.032 (8)	0.033 (7)	0.031 (6)	0.012 (4)	0.012 (6)	0.020 (5)

Geometric parameters (Å, º)

Zn1—O1	1.929 (19)	N13—H13C	0.8500
Zn1—O14^i	2.01 (7)	N13—C13	1.46 (4)
Zn1—O4^ii	1.953 (18)	N3—H3A	0.8900
Zn1—O11	1.93 (5)	N3—H3B	0.8000
O1—C1	1.28 (4)	N3—H3C	0.8500
O2—C1	1.24 (2)	N3—C3	1.44 (2)
O14—C14	1.27 (2)	C2—H2A	0.9700
O4—C4	1.29 (3)	C2—H2B	0.9700
O11—C11	1.25 (3)	C2—C1	1.52 (3)
O1W—H1WA	0.8567	C2—C3	1.56 (2)
O1W—H1WB	0.8493	C4—C3	1.50 (3)
O13—C14	1.30 (3)	C14—C13	1.53 (4)
O3—C4	1.25 (2)	C11—C12	1.48 (3)
O12—C11	1.22 (2)	C12—H12A	0.9700
O2W—H2WA	0.8221	C12—H12B	0.9700
O2W—H2WB	0.8340	C12—C13	1.42 (4)
N13—H13A	0.8700	C13—H13	0.9800
N13—H13B	0.8700	C3—H3	0.9800
O1—Zn1—O14^i	113.7 (18)	O4—C4—C3	114.8 (13)
O1—Zn1—O4^ii	98.6 (9)	O3—C4—O4	124 (3)
O1—Zn1—O11	111 (2)	O3—C4—C3	120.3 (17)
O4^ii—Zn1—O14^i	102.1 (16)	O14—C14—O13	115 (4)
O11—Zn1—O14^i	121 (2)	O14—C14—C13	116 (4)
O11—Zn1—O4^ii	106.4 (18)	O13—C14—C13	129 (3)
C1—O1—Zn1	136 (4)	O11—C11—C12	111.0 (14)
C14—O14—Zn1^i	111 (3)	O12—C11—O11	125 (3)
C4—O4—Zn1^ii	123.2 (10)	O12—C11—C12	123.9 (18)
C11—O11—Zn1	129 (3)	C11—C12—H12A	107.2
H1WA—O1W—H1WB	104.2	C11—C12—H12B	107.2
H2WA—O2W—H2WB	106.0	H12A—C12—H12B	106.8
H13A—N13—H13B	109.5	C13—C12—C11	121 (3)
H13A—N13—H13C	111.0	C13—C12—H12A	107.2
H13B—N13—H13C	109.5	C13—C12—H12B	107.2
C13—N13—H13A	109.5	N13—C13—C14	106 (4)
C13—N13—H13B	105.0	N13—C13—H13	115.0
C13—N13—H13C	112.0	C14—C13—H13	108.9
H3A—N3—H3B	113.0	C12—C13—N13	117 (3)
H3A—N3—H3C	107.0	C12—C13—C14	107 (4)
H3B—N3—H3C	114.0	C12—C13—H13	108.9
C3—N3—H3A	111.0	O1—C1—C2	116 (3)
C3—N3—H3B	105.0	O2—C1—O1	122 (4)
C3—N3—H3C	107.0	O2—C1—C2	122 (3)
H2A—C2—H2B	107.9	N3—C3—C2	112.6 (19)
C1—C2—H2A	109.2	N3—C3—C4	108 (3)
C1—C2—H2B	109.2	N3—C3—H3	112.0
C1—C2—C3	112.2 (16)	C2—C3—H3	106.2
C3—C2—H2A	109.2	C4—C3—C2	113.3 (16)
C3—C2—H2B	109.2	C4—C3—H3	106.2
Zn1—O1—C1—C2	15 (3)	N13—C13—C14—O13	14 (4)
Zn1—O14^i—C14^i—C13^i	173.0 (18)	N3—C3—C4—O3	−22 (5)
Zn1—O4^ii—C4^ii—C3^ii	−174 (3)	C11—C12—C13—N13	58 (8)
Zn1—O11—C11—C12	157 (5)	C11—C12—C13—C14	−60 (5)
O2—C1—C2—C3	25 (3)	C1—C2—C3—N3	−61 (4)
O12—C11—C12—C13	154 (6)	C1—C2—C3—C4	60 (2)

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

(Zn-aspartate_dihydrate_3_05GPa)

Crystal data

C16H24N4O16Zn2·4(H2O)	Z = 1
Mr = 731.19	F(000) = 376
Triclinic, P1	Dx = 2.069 Mg m^−3
a = 8.415 (4) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.033 (4) Å	Cell parameters from 327 reflections
c = 9.5778 (17) Å	θ = 4.0–27.4°
α = 110.49 (3)°	µ = 2.16 mm^−1
β = 104.77 (3)°	T = 296 K
γ = 108.92 (5)°	Plate, colourless
V = 586.8 (5) Å^3	0.25 × 0.20 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.065
Radiation source: sealed x-ray tube	θmax = 27.4°, θmin = 4.0°
ω scan	h = −4→4
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −8→8
Tmin = 0.608, Tmax = 0.900	l = −12→12
2377 measured reflections	12 standard reflections every 84 reflections
440 independent reflections	intensity decay: none
327 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.036	H-atom parameters constrained
wR(F^2) = 0.085	w = 1/[σ^2(Fo^2) + (0.0544P)^2 + 0.3153P] where P = (Fo^2 + 2Fc^2)/3
S = 1.07	(Δ/σ)max < 0.001
440 reflections	Δρmax = 0.21 e Å^−3
198 parameters	Δρmin = −0.15 e Å^−3
126 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 3.05 (2) GPa (3050000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.6965 (14)	0.3198 (7)	0.5275 (2)	0.043 (13)
O1	0.634 (3)	0.3435 (17)	0.7156 (9)	0.039 (4)
O2	0.584 (3)	0.2830 (17)	0.9065 (9)	0.036 (6)
O14	1.109 (8)	0.759 (4)	0.4868 (19)	0.053 (8)
O4	0.527 (3)	−0.1049 (16)	0.6418 (8)	0.033 (4)
O11	0.701 (5)	0.509 (3)	0.4835 (9)	0.031 (5)
O1W	0.241 (4)	0.0350 (18)	0.7780 (9)	0.032 (6)
H1WA	0.352455	0.107109	0.808728	0.047*
H1WB	0.213022	−0.047092	0.684478	0.047*
O13	0.942 (4)	0.508 (2)	0.2613 (12)	0.043 (7)
O3	0.513 (3)	−0.1641 (15)	0.8470 (8)	0.037 (6)
O12	0.825 (4)	0.737 (2)	0.7302 (9)	0.038 (6)
O2W	0.232 (3)	0.3211 (17)	1.0127 (9)	0.038 (6)
H2WA	0.204770	0.223193	0.933353	0.057*
H2WB	0.254475	0.304054	1.095837	0.057*
N13	0.628 (2)	0.526 (2)	0.215 (17)	0.0290 (3)
H13A	0.636167	0.482799	0.121891	0.035*
H13B	0.539355	0.554456	0.201408	0.035*
H13C	0.608602	0.450977	0.249310	0.035*
N3	0.802 (5)	0.1559 (19)	1.0631 (10)	0.038 (7)
H3A	0.711687	0.201226	1.064078	0.038*
H3B	0.894515	0.228842	1.117093	0.038*
H3C	0.756227	0.072026	1.082374	0.038*
C4	0.603 (5)	−0.083 (2)	0.7892 (12)	0.029 (5)
C13	0.811 (6)	0.701 (3)	0.3404 (19)	0.026 (8)
H13	0.842274	0.790701	0.303282	0.031*
C11	0.768 (5)	0.676 (3)	0.5814 (13)	0.030 (5)
C12	0.800 (5)	0.783 (2)	0.4960 (12)	0.029 (5)
H12A	0.702236	0.817163	0.477437	0.035*
H12B	0.914931	0.890891	0.568785	0.035*
C14	0.967 (6)	0.643 (3)	0.361 (2)	0.025 (8)
C3	0.783 (4)	0.081 (2)	0.8977 (12)	0.032 (5)
H3	0.879972	0.043506	0.897901	0.038*
C2	0.820 (5)	0.221 (2)	0.838 (2)	0.034 (7)
H2A	0.937743	0.322825	0.915356	0.041*
H2B	0.827963	0.171389	0.733532	0.041*
C1	0.670 (4)	0.282 (2)	0.817 (2)	0.022 (6)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.05 (2)	0.038 (4)	0.0299 (9)	0.003 (9)	0.007 (3)	0.0193 (14)
O1	0.042 (7)	0.043 (5)	0.036 (4)	0.018 (3)	0.017 (5)	0.022 (4)
O2	0.037 (11)	0.041 (7)	0.035 (4)	0.015 (6)	0.019 (7)	0.023 (4)
O14	0.052 (10)	0.052 (9)	0.053 (8)	0.029 (5)	0.018 (6)	0.019 (5)
O4	0.035 (6)	0.034 (5)	0.031 (3)	0.015 (3)	0.014 (5)	0.018 (4)
O11	0.033 (7)	0.032 (5)	0.028 (4)	0.018 (4)	0.011 (5)	0.014 (4)
O1W	0.029 (11)	0.027 (6)	0.035 (4)	0.016 (6)	0.009 (7)	0.011 (5)
O13	0.035 (12)	0.040 (7)	0.045 (5)	0.020 (6)	0.013 (8)	0.011 (5)
O3	0.038 (11)	0.034 (6)	0.038 (4)	0.013 (6)	0.014 (7)	0.021 (4)
O12	0.041 (11)	0.048 (7)	0.029 (4)	0.023 (6)	0.016 (7)	0.018 (5)
O2W	0.042 (11)	0.043 (7)	0.032 (4)	0.022 (6)	0.011 (7)	0.022 (4)
N13	0.034 (12)	0.033 (7)	0.028 (5)	0.018 (6)	0.009 (9)	0.016 (5)
N3	0.034 (12)	0.027 (7)	0.045 (5)	0.015 (6)	−0.002 (8)	0.022 (6)
C4	0.031 (7)	0.030 (6)	0.028 (5)	0.015 (4)	0.010 (5)	0.015 (5)
C13	0.025 (10)	0.025 (9)	0.027 (8)	0.011 (5)	0.010 (6)	0.013 (6)
C11	0.032 (7)	0.032 (6)	0.030 (5)	0.012 (4)	0.014 (5)	0.017 (5)
C12	0.031 (7)	0.027 (6)	0.031 (5)	0.014 (4)	0.010 (5)	0.017 (4)
C14	0.025 (10)	0.024 (9)	0.026 (8)	0.012 (5)	0.010 (6)	0.010 (6)
C3	0.031 (7)	0.032 (6)	0.032 (5)	0.013 (4)	0.014 (5)	0.016 (5)
C2	0.035 (9)	0.033 (8)	0.035 (7)	0.015 (4)	0.013 (6)	0.019 (6)
C1	0.022 (8)	0.020 (7)	0.024 (7)	0.009 (4)	0.008 (6)	0.012 (5)

Geometric parameters (Å, º)

Zn1—O1	1.962 (15)	N13—H13C	0.8400
Zn1—O14^i	2.01 (7)	N13—C13	1.48 (3)
Zn1—O4^ii	1.954 (11)	N3—H3A	0.9700
Zn1—O11	1.89 (4)	N3—H3B	0.7300
O1—C1	1.30 (3)	N3—H3C	0.8400
O2—C1	1.26 (3)	N3—C3	1.431 (19)
O14—C14	1.25 (3)	C4—C3	1.493 (18)
O4—C4	1.31 (2)	C13—H13	0.9800
O11—C11	1.29 (3)	C13—C12	1.45 (3)
O1W—H1WA	0.8502	C13—C14	1.56 (4)
O1W—H1WB	0.8504	C11—C12	1.476 (19)
O13—C14	1.17 (4)	C12—H12A	0.9700
O3—C4	1.249 (18)	C12—H12B	0.9700
O12—C11	1.224 (13)	C3—H3	0.9800
O2W—H2WA	0.8492	C3—C2	1.54 (2)
O2W—H2WB	0.8499	C2—H2A	0.9700
N13—H13A	0.8700	C2—H2B	0.9700
N13—H13B	0.8600	C2—C1	1.53 (4)
O1—Zn1—O14^i	117.2 (12)	C12—C13—H13	107.7
O4^ii—Zn1—O1	98.4 (7)	C12—C13—C14	111 (3)
O4^ii—Zn1—O14^i	101.3 (13)	C14—C13—H13	107.7
O11—Zn1—O1	109.6 (17)	O11—C11—C12	111.7 (10)
O11—Zn1—O14^i	119.3 (18)	O12—C11—O11	123 (2)
O11—Zn1—O4^ii	108.0 (13)	O12—C11—C12	124.5 (13)
C1—O1—Zn1	130 (2)	C13—C12—C11	117 (3)
C14—O14—Zn1^i	105 (4)	C13—C12—H12A	108.0
C4—O4—Zn1^ii	122.0 (6)	C13—C12—H12B	108.0
C11—O11—Zn1	130.6 (13)	C11—C12—H12A	108.0
H1WA—O1W—H1WB	104.4	C11—C12—H12B	108.0
H2WA—O2W—H2WB	104.6	H12A—C12—H12B	107.2
H13A—N13—H13B	109.5	O14—C14—C13	111 (4)
H13A—N13—H13C	109.5	O13—C14—O14	129 (6)
H13B—N13—H13C	109.5	O13—C14—C13	120 (3)
C13—N13—H13A	109.5	N3—C3—C4	111.0 (14)
C13—N13—H13B	107.0	N3—C3—H3	106.5
C13—N13—H13C	111.0	N3—C3—C2	111.5 (16)
H3A—N3—H3B	109.5	C4—C3—H3	106.5
H3A—N3—H3C	100.0	C4—C3—C2	114.4 (12)
H3B—N3—H3C	122.0	C2—C3—H3	106.5
C3—N3—H3A	106.0	C3—C2—H2A	109.0
C3—N3—H3B	109.5	C3—C2—H2B	109.0
C3—N3—H3C	108.0	H2A—C2—H2B	107.8
O4—C4—C3	114.8 (9)	C1—C2—C3	113.0 (18)
O3—C4—O4	122 (2)	C1—C2—H2A	109.0
O3—C4—C3	121.2 (9)	C1—C2—H2B	109.0
N13—C13—H13	114.0	O1—C1—C2	123 (2)
N13—C13—C14	107 (3)	O2—C1—O1	117 (4)
C12—C13—N13	115 (3)	O2—C1—C2	120 (3)
Zn1—O1—C1—C2	18.1 (19)	N13—C13—C14—O13	20 (6)
Zn1—O14^i—C14^i—C13^i	170.9 (12)	N3—C3—C4—O3	−18 (4)
Zn1—O4^ii—C4^ii—C3^ii	−174 (2)	C11—C12—C13—N13	64 (5)
Zn1—O11—C11—C12	160 (4)	C11—C12—C13—C14	−58 (3)
O2—C1—C2—C3	30 (2)	C1—C2—C3—N3	−69 (3)
O12—C11—C12—C13	150 (4)	C1—C2—C3—C4	58 (2)

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

(Zn-aspartate_dihydrate_3_53GPa)

Crystal data

C16H24N4O16Zn2·4(H2O)	Z = 1
Mr = 731.19	F(000) = 376
Triclinic, P1	Dx = 2.092 Mg m^−3
a = 8.386 (5) Å	Mo Kα radiation, λ = 0.71073 Å
b = 8.983 (3) Å	Cell parameters from 284 reflections
c = 9.5498 (19) Å	θ = 4.1–27.4°
α = 110.18 (2)°	µ = 2.18 mm^−1
β = 104.73 (3)°	T = 296 K
γ = 109.15 (4)°	Plate, colourless
V = 580.5 (5) Å^3	0.25 × 0.20 × 0.05 mm

Data collection

Multiwire proportional diffractometer	Rint = 0.084
Radiation source: sealed x-ray tube	θmax = 27.4°, θmin = 4.1°
ω scan	h = −5→4
Absorption correction: integration Correction for absorption was made using XEMP (SHELXTL, Sheldrick (2015).	k = −8→8
Tmin = 0.599, Tmax = 0.897	l = −12→11
2344 measured reflections	12 standard reflections every 84 reflections
421 independent reflections	intensity decay: none
284 reflections with I > 2σ(I)

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.054	H-atom parameters constrained
wR(F^2) = 0.163	w = 1/[σ^2(Fo^2) + (0.1189P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.13	(Δ/σ)max < 0.001
421 reflections	Δρmax = 0.43 e Å^−3
198 parameters	Δρmin = −0.29 e Å^−3
126 restraints

Special details

Experimental. Data were collected at room temperature and pressure of 3.53 (2) GPa (3530000 kPa) with the crystal obtained by the in-situ high-pressure crystallization technique. Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.6859 (17)	0.3227 (10)	0.5251 (4)	0.066 (17)
O1	0.636 (5)	0.345 (3)	0.7162 (15)	0.042 (5)
O2	0.598 (5)	0.282 (3)	0.9093 (14)	0.039 (8)
O14	1.125 (9)	0.746 (5)	0.486 (2)	0.021 (7)
O4	0.536 (6)	−0.104 (3)	0.6453 (14)	0.031 (5)
O11	0.710 (8)	0.507 (4)	0.4821 (15)	0.041 (6)
O1W	0.239 (6)	0.036 (3)	0.7777 (16)	0.043 (8)
H1WA	0.354154	0.103369	0.817840	0.065*
H1WB	0.213955	−0.037761	0.681240	0.065*
O13	0.944 (7)	0.506 (4)	0.2630 (19)	0.045 (8)
O3	0.523 (5)	−0.166 (3)	0.8474 (13)	0.042 (8)
O12	0.836 (6)	0.732 (4)	0.7292 (15)	0.042 (8)
O2W	0.226 (5)	0.324 (3)	1.0150 (15)	0.040 (8)
H2WA	0.240072	0.236654	0.969367	0.061*
H2WB	0.233859	0.333204	1.106321	0.061*
N13	0.6283 (2)	0.526 (2)	0.216 (2)	0.035 (7)
H13A	0.636167	0.482799	0.121891	0.035*
H13B	0.539355	0.554456	0.201408	0.035*
H13C	0.608602	0.450977	0.249310	0.035*
N3	0.7820 (2)	0.15150 (18)	1.05345 (17)	0.041 (7)
H3A	0.711687	0.201226	1.064078	0.038*
H3B	0.894515	0.228842	1.117093	0.038*
H3C	0.756227	0.072026	1.082374	0.038*
C4	0.600 (6)	−0.082 (3)	0.7879 (18)	0.031 (6)
C13	0.820 (10)	0.703 (5)	0.341 (3)	0.025 (10)
H13	0.858374	0.792701	0.304345	0.030*
C11	0.762 (8)	0.680 (5)	0.581 (2)	0.031 (6)
C12	0.802 (8)	0.788 (4)	0.4936 (19)	0.031 (6)
H12A	0.702412	0.820892	0.468608	0.037*
H12B	0.915326	0.897887	0.568166	0.037*
C14	0.970 (10)	0.638 (6)	0.364 (4)	0.043 (14)
C3	0.785 (6)	0.083 (4)	0.8984 (19)	0.034 (6)
H3	0.878002	0.040906	0.889884	0.041*
C2	0.822 (7)	0.223 (4)	0.836 (3)	0.036 (11)
H2A	0.942306	0.324716	0.911152	0.043*
H2B	0.826625	0.171181	0.729821	0.043*
C1	0.671 (7)	0.286 (3)	0.818 (3)	0.031 (11)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.06 (2)	0.063 (8)	0.0384 (16)	−0.011 (13)	0.010 (4)	0.027 (2)
O1	0.046 (8)	0.043 (7)	0.039 (5)	0.021 (4)	0.018 (5)	0.021 (5)
O2	0.046 (12)	0.041 (9)	0.036 (6)	0.016 (6)	0.016 (8)	0.028 (6)
O14	0.019 (9)	0.020 (8)	0.022 (7)	0.011 (5)	0.008 (6)	0.006 (5)
O4	0.031 (7)	0.029 (6)	0.031 (5)	0.016 (4)	0.010 (5)	0.013 (5)
O11	0.042 (8)	0.041 (7)	0.039 (6)	0.020 (4)	0.015 (6)	0.020 (5)
O1W	0.049 (12)	0.044 (9)	0.038