Syntheses and crystal structures of three novel oxalate coordination compounds: Rb2Co(C2O4)2·4H2O, Rb2CoCl2(C2O4) and K2Li2Cu(C2O4)3·2H2O

Clulow, R.; Lightfoot, P.

doi:10.1107/S2056989023001822

research communications

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ISSN: 2056-9890

Volume 79| Part 4| April 2023| Pages 267-271

https://doi.org/10.1107/S2056989023001822

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Syntheses and crystal structures of three novel oxalate coordination compounds: Rb₂Co(C₂O₄)₂·4H₂O, Rb₂CoCl₂(C₂O₄) and K₂Li₂Cu(C₂O₄)₃·2H₂O

Rebecca Clulow ^a,^b ^* and Philip Lightfoot ^b

^aDepartment of Chemistry - Ångström Laboratory, Lägerhyddsvägen 1, Box 538, 751 21, Uppsala, Sweden, and ^bSchool of Chemistry, University of St Andrews, KY16 9ST, Scotland, United Kingdom
^*Correspondence e-mail: rebecca.clulow@kemi.uu.se

Edited by M. Weil, Vienna University of Technology, Austria (Received 15 December 2022; accepted 27 February 2023; online 7 March 2023)

Single crystals of three novel transition-metal oxalates, dirubidium diaquadioxalatocobalt(II) dihydrate or dirubidium cobalt(II) bis(oxalate) tetrahydrate, Rb₂[Co(C₂O₄)₂(H₂O)₂]·2H₂O, (I), catena-poly[dirubidium [[dichloridocobalt(II)]-μ-oxalato]] or dirubidium cobalt(II) dichloride oxalate, {Rb₂[CoCl₂(C₂O₄)]}_n, (II), and poly[dipotassium [tri-μ-oxalato-copper(II)dilithium] dihydrate] or dipotassium dilithium copper(II) tris(oxalate) dihydrate, {K₂[Li₂Cu(C₂O₄)₃]·2H₂O}_n, (III), have been grown under hydrothermal conditions and their crystal structures determined using single-crystal X-ray diffraction. The structure of (I) exhibits isolated octahedral [Co(C₂O₄)₂(H₂O)₂] units, whereas (II) consists of trans chains of Co²⁺ ions bridged by bidentate oxalato ligands and (III) displays a novel tri-periodic network of Li⁺ and Cu²⁺ ions linked by oxalato bridging ligands.

Keywords: crystal structure; oxalates; coordination compounds; first-row transition metals.

CCDC references: 2245039; 2245038; 2245037

1. Chemical context

Oxalate-based transition-metal complexes have long attracted interest because of their promising magnetic and electrochemical properties. Their magnetic properties are in part due to the oxalato ligand, which is known to facilitate magnetic exchange between transition-metal cations, and the compounds are known to exhibit both ferro- and antiferromagnetic interactions (Miller & Drillon, 2002 ; Baran, 2014 ). In addition to their magnetic properties, there have also been numerous studies concerning their electrochemical properties, which have shown promising results (Pramanik et al., 2022 ; Cai et al., 2020 ; Yao et al., 2019 ). Part of the appeal of oxalate-based coordination compounds is due to their high degree of structural diversity, as a result of the oxalate ligand, which can adopt 17 different coordination modes and act as a mono-, bi-, tri- or tetradentate ligand (Rao et al., 2004 ). This has led to a vast compositional area, which is yet to be fully explored. In this context, the crystal structures of three new oxalate-based coordination compounds are reported and discussed herein.

2. Structural commentary

Rb₂Co(C₂O₄)₂·4H₂O (I) consists of isolated [Co(C₂O₄)₂(H₂O)₂] octahedra. The Co²⁺ cation lies on the 2c Wyckoff position with a site symmetry of $[\overline{1}]$ , leading to a trans disposition of the bidentate oxalato and aqua ligands (Fig. 1). The average Co—O bond length was determined as 2.080 Å, with a calculated bond-valence sum of 2.10 valence units. The Rb⁺ cation has a coordination number of 11, defined by oxalate O atoms and water molecules. While the water molecule involving O1 coordinates to both Rb⁺ and Co²⁺, the second water molecule involving O2 solely bonds to the alkali metal cation. The [Co(C₂O₄)₂(H₂O)₂] octahedra are interlinked by hydrogen bonding of both types of water molecules, as shown in Fig. 2. The mutually trans coordinating water molecules (H3, O1, H4) form hydrogen bonds with the oxalate ligands of the neighbouring [Co(C₂O₄)₂(H₂O)₂] octahedra, whilst the second type of water molecule (H1, O2, H2) forms hydrogen bonds (in part bifurcated) with the oxalate ligands of two separate [Co(C₂O₄)₂(H₂O)₂] octahedra. Numerical data for the hydrogen-bonding interactions are given in Table 1.

Table 1
Hydrogen-bond geometry (Å, °) for (I)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2—H1⋯O4	0.89 (4)	2.00 (4)	2.880 (2)	171 (4)
O2—H2⋯O4ⁱ	0.85 (5)	2.47 (5)	3.187 (2)	143 (4)
O2—H2⋯O6ⁱ	0.85 (5)	2.20 (5)	3.008 (2)	159 (4)
O1—H3⋯O5ⁱⁱ	0.76 (3)	1.98 (3)	2.736 (2)	174 (3)
O1—H4⋯O6ⁱⁱⁱ	0.78 (3)	2.05 (3)	2.825 (2)	172 (3)
Symmetry codes: (i) ; (ii) $[-x+{\script{3\over 2}}, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (iii) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ .

Figure 1
Coordination environment of Co²⁺ in Rb₂Co(C₂O₄)₂·4H₂O (I). Colour code: Co (blue), C (black), O (red) and H (light pink). Displacement ellipsoids are drawn at the 50% probability level. [Symmetry code: (viii) −x + 1, −y, −z + 1].

Figure 2
The hydrogen-bonding network of Rb₂Co(C₂O₄)₂·2H₂O (I) viewed along the a and b axes. Displacement ellipsoids are drawn at the 30% probability level. The hydrogen bonds are shown as dashed lines. Colour code: Rb (pink), Co (blue), C (black), O (red) and H (light pink).

Rb₂CoCl₂(C₂O₄) (II) consists of octahedrally coordinated Co²⁺ cations. They are linked by bis-bidentate oxalate ligands to form chains extending parallel to the a axis, as shown in Fig. 3. The oxalate ligands are mutually trans to one another whilst the Cl⁻ anions cap each side of the octahedron. Co—O bond lengths are 2.0616 (17) Å and longer for the Co—Cl bond at 2.4863 (9) Å, with a calculated bond-valence sum of 2.03 valence units for Co. The Rb⁺ cation has a coordination number of eight and lies between the layers formed by the Co²⁺ chains (Fig. 4), with no direct connectivity between the chains. Each of the atoms lies on a special position within the unit cell with Wyckoff positions/site symmetries: Rb⁺ (4i, mm2), Co²⁺ (2d, mmm), Cl⁻ (4j, mm2), O (8n,. .m) and C (4h, m2m). The presence of the oxalate-bridged Co²⁺ chain could allow for magnetic exchange (García-Couceiro et al., 2004 ), hence the magnetic properties of the compound should also be investigated in the future.

Figure 3
Coordination environment of Co²⁺ in Rb₂CoCl₂(C₂O₄) (II). Colour code: Co (blue), Cl (green), C (black) and O (red). Displacement ellipsoids are drawn at 50% probability level. [Symmetry codes: (i) −x + 1, y, −z + 1; (vii) x, −y + 2, z; (viii) −x + 1, −y + 2, −z + 1; (ix) −x + 2, −y + 2, −z + 1; (xii) x − 1, y, z].

Figure 4
The crystal structure of Rb₂CoCl₂(C₂O₄) (II) in a view approximately along the a axis.

The Cu²⁺ and Li⁺ binding environments of K₂Li₂Cu(C₂O₄)₃·2H₂O (III) are shown in Fig. 5. The d⁹ Cu²⁺ cations display classic Jahn–Teller distortion with elongation of the axial Cu—O bonds. The equatorial Cu—O bond lengths are 1.938 (3) (O2) and 1.942 (3) (O1) Å whilst the axial bonds are significantly longer at 2.473 (4) Å (O6). The Cu²⁺ ion lies on a special position with Wyckoff position and site symmetry of 6b and $[\overline{3}]$ , respectively. The Cu²⁺ coordination environment consists of four oxalate ligands, two of which act as bidentate bridging ligands and two of which are axially oriented and bind to four metal cations with a tricoordinate oxygen atom. The Li⁺ cation is tetrahedrally coordinated by three oxalate molecules, one of which is bidentate whilst the other two are monodentate. The Cu²⁺ and Li⁺-centred polyhedra are interconnected into a tri-periodic network, as shown in Fig. 6. The coordination environment of the K⁺ cation lies within this network and consists of eight oxygen atoms from the oxalate ligands and two water molecules. These water molecules exhibit disorder of the O7 atom, which is split into two positions. The interatomic distances between the water molecules is ∼3.7 Å, which is too far apart to facilitate hydrogen bonding.

Figure 5
Coordination environments of Cu²⁺ and of Li⁺ in the crystal structure of K₂Li₂Cu(C₂O₄)₃·2H₂O (III). Colour code: Li (green), Cu (Blue), C (black) and O (red). Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (i) −x + 2, −y + 2, −z + 2; (vii) −x, −y, −z + 1; (ix) x + 1, y + 1, z; (xi) x − 1, y, z; (xii) −x + 1, −y + 1, −z + 1; (xiii) x + 1, y + 1, z + 1].

Figure 6
The crystal structure of K₂Li₂Cu(C₂O₄)₃·2H₂O (III) viewed along the a axis.

3. Database survey

Database surveys were carried out using the Cambridge Structural Database (CSD, last update November 2022; Groom et al., 2016 ) for compounds with structural similarities to the three new oxalate coordination compounds reported here. For (I), a search for first-row transition metals with the same coordination environment produced numerous results for a range of transition metals. The most similar is DIHXID [dipotassium bis(oxalato)diaquacobalt(II) tetrahydrate; Chylewska et al., 2013 ), which has the same formula type and coordination environment as (I) although with K⁺ rather Rb⁺ cations, but is not isostructural. For (II), there are several compounds containing transition-metal oxalate chains with the same binding environment, although with quite different cations involved. For example BEJHOQ {catena-[bis(2-(5,6-dihydro-2H-[1,3]dithiolo[4,5-b][1,4]dithiin-2-ylidene)-5,6-dihydro-2H-[1,3]dithiolo[4,5-b][1,4]dithiin-1-ium) bis(μ-oxalato)tetrachlorodiiron(III) dichloromethane solvate]} and EYALIB {catena-[bis(2-(5,6-dihydro-2H-[1,3]diselenolo[4,5-b][1,4]dithiin-2-ylidene)-5,6-dihydro-2H-[1,3]diselenolo[4,5-b][1,4]dithiin-1-ium) bis(μ-oxalato)tetrachlorodiiron(III)]; Zhang, 2016 , 2017 ). The database survey of compounds with similar binding environments to (III) focused on first-row transition metals with two bidentate and two mutually trans monodentate oxalate ligands, containing a tricoordinating oxygen atom. The search revealed evidence of only two similar compounds, viz. ADAJUL [octaammonium hexakis(μ₂-oxalato-O,O,O′)bis(oxalato-O,O′)diaquatetracopper(II) tetrahydrate] and ASOXOV {bis[1,4-diazoniabicyclo(2.2.2)octane]bis(μ₂-oxalato)diaquabis(oxalato)dicopper(II) tetrahydrate; Kadir et al., 2006 ; Keene et al., 2004 }. These contain similar types of linkages, although with only one type of cation and only as discrete molecules rather than coordination polymers. Hence, (III) represents the first example of this type of binding environment.

4. Synthesis and crystallization

The samples were synthesized via hydrothermal syntheses in the temperature range 433–463 K over four days, from commercially available starting reagents. Compounds (I) and (II) were synthesized as by-products from the reaction of rubidium carbonate, sodium carbonate, cobalt chloride hexahydrate and oxalic acid dihydrate in molar ratios of 2:2:1:1.5 and 1:1.5:1:1.5 at 433 and 463 K, respectively. Compound (III) was synthesized by the reaction of potassium carbonate, lithium carbonate, copper chloride dihydrate and oxalic acid dihydrate (1:3:1:3) at 463 K. Single crystals were isolated from a mixture of products for further analysis. The resulting crystals were filtered and dried overnight at 323 K prior to analysis by X-ray diffraction.

5. Refinement

Crystal data and refinement details of the three compounds are summarized in Table 2. The H atoms in (I) and (III) were allowed to refine freely. The disordered oxygen atom in compound III (O7) was split over two positions with their occupancies fixed at 0.5 while their atomic coordinates and U^ijs were refined independently.

Table 2
Experimental details

	(I)	(II)	(III)
Crystal data
Chemical formula	Rb₂[Co(C₂O₄)₂(H₂O)₂]·2H₂O	Rb₂[CoCl₂(C₂O₄)]	K₂[Li₂Cu(C₂O₄)₃]·2H₂O
M_r	477.97	388.79	455.71
Crystal system, space group	Monoclinic, P2₁/n	Orthorhombic, Immm	Triclinic, P $[\overline{1}]$
Temperature (K)	173	173	173
a, b, c (Å)	7.8434 (5), 7.0795 (4), 10.9133 (7)	5.3445 (3), 6.4380 (4), 12.5866 (8)	6.1847 (4), 7.2575 (5), 8.1795 (5)
α, β, γ (°)	90, 102.836 (8), 90	90, 90, 90	101.327 (11), 91.723 (11), 113.563 (11)
V (Å³)	590.84 (7)	433.08 (5)	327.56 (5)
Z	2	2	1
Radiation type	Mo Kα	Mo Kα	Mo Kα
μ (mm⁻¹)	9.70	13.73	2.39
Crystal size (mm)	0.21 × 0.16 × 0.08	0.20 × 0.15 × 0.07	0.14 × 0.14 × 0.07

Data collection
Diffractometer	Rigaku Mercury2 (2x2 bin mode)	Rigaku Mercury2 (2x2 bin mode)	Rigaku Mercury2 (2x2 bin mode)
Absorption correction	Multi-scan (SADABS; Krause et al., 2015 )	Multi-scan (SADABS; Krause et al., 2015)	Multi-scan (SADABS; Krause et al., 2015)
T_min, T_max	0.681, 1.00	0.671, 1.00	0.610, 1.00
No. of measured, independent and observed [I > 2σ(I)] reflections	5799, 1343, 1169	2218, 310, 296	3403, 1500, 1077
R_int	0.039	0.034	0.095
(sin θ/λ)_max (Å⁻¹)	0.650	0.649	0.651

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.021, 0.050, 0.97	0.018, 0.043, 1.11	0.045, 0.114, 0.94
No. of reflections	1343	310	1500
No. of parameters	104	22	132
H-atom treatment	All H-atom parameters refined	–	All H-atom parameters refined
Δρ_max, Δρ_min (e Å⁻³)	0.65, −0.64	0.63, −0.53	1.03, −1.01
Computer programs: CrystalClear (Rigaku, 2015 ), SHELXT (Sheldrick, 2015a ), SHELXL (Sheldrick, 2015b ) and ORTEP for Windows and WinGX (Farrugia, 2012 ).

Supporting information

CCDC references: 2245039; 2245038; 2245037

Crystal structure: contains datablocks I, II, III, global. DOI: https://doi.org/10.1107/S2056989023001822/wm5668sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989023001822/wm5668Isup2.hkl

Structure factors: contains datablock II. DOI: https://doi.org/10.1107/S2056989023001822/wm5668IIsup3.hkl

Structure factors: contains datablock III. DOI: https://doi.org/10.1107/S2056989023001822/wm5668IIIsup4.hkl

checkCIF report

Computing details top

For all structures, data collection: CrystalClear (Rigaku, 2015); cell refinement: CrystalClear (Rigaku, 2015); data reduction: CrystalClear (Rigaku, 2015); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL (Sheldrick, 2015b); molecular graphics: ORTEP for Windows (Farrugia, 2012); software used to prepare material for publication: WinGX (Farrugia, 2012).

Dirubidium diaquadioxalatocobalt(II) dihydrate (I) top

Crystal data top

Rb₂[Co(C₂O₄)₂(H₂O)₂]·2H₂O	F(000) = 458
M_r = 477.97	D_x = 2.687 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71075 Å
Hall symbol: -P 2yn	Cell parameters from 935 reflections
a = 7.8434 (5) Å	θ = 1.9–27.5°
b = 7.0795 (4) Å	µ = 9.70 mm⁻¹
c = 10.9133 (7) Å	T = 173 K
β = 102.836 (8)°	Prism, orange
V = 590.84 (7) Å³	0.21 × 0.16 × 0.08 mm
Z = 2

Data collection top

Rigaku Mercury2 (2x2 bin mode) diffractometer	1343 independent reflections
Radiation source: Sealed Tube	1169 reflections with I > 2σ(I)
Detector resolution: 13.6612 pixels mm^-1	R_int = 0.039
profile data from ω–scans	θ_max = 27.5°, θ_min = 2.9°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −10→10
T_min = 0.681, T_max = 1.00	k = −9→9
5799 measured reflections	l = −14→13

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F² > 2σ(F²)] = 0.021	All H-atom parameters refined
wR(F²) = 0.050	w = 1/[σ²(F_o²) + (0.0323P)²] where P = (F_o² + 2F_c²)/3
S = 0.97	(Δ/σ)_max < 0.001
1343 reflections	Δρ_max = 0.65 e Å⁻³
104 parameters	Δρ_min = −0.64 e Å⁻³

Special details top

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

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

	x	y	z	U_iso*/U_eq
Rb1	0.81534 (3)	0.66030 (3)	0.37962 (2)	0.01935 (9)
Co1	0.500000	0.000000	0.500000	0.01014 (11)
O1	0.5165 (2)	0.2912 (2)	0.49112 (17)	0.0160 (3)
O2	0.8705 (2)	0.2408 (3)	0.39553 (17)	0.0236 (4)
O3	0.50631 (18)	0.0198 (2)	0.69060 (13)	0.0143 (3)
O4	0.77067 (18)	−0.0152 (2)	0.57235 (13)	0.0139 (3)
O5	0.6916 (2)	−0.0314 (2)	0.87422 (14)	0.0186 (3)
O6	0.96271 (19)	0.0330 (2)	0.75326 (14)	0.0191 (3)
C1	0.6578 (3)	−0.0014 (3)	0.75938 (19)	0.0118 (4)
C2	0.8121 (3)	0.0076 (3)	0.69128 (19)	0.0122 (4)
H1	0.828 (5)	0.168 (5)	0.449 (4)	0.056 (11)*
H2	0.942 (6)	0.173 (6)	0.367 (4)	0.079 (15)*
H3	0.594 (4)	0.342 (4)	0.532 (3)	0.023 (8)*
H4	0.494 (4)	0.345 (4)	0.427 (3)	0.029 (9)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Rb1	0.01880 (14)	0.02412 (14)	0.01580 (13)	0.00190 (8)	0.00529 (9)	0.00010 (8)
Co1	0.0105 (2)	0.01303 (19)	0.00658 (19)	0.00024 (14)	0.00112 (15)	−0.00043 (14)
O1	0.0195 (9)	0.0142 (7)	0.0118 (8)	−0.0033 (6)	−0.0020 (7)	0.0004 (6)
O2	0.0248 (10)	0.0268 (9)	0.0231 (9)	−0.0002 (8)	0.0138 (8)	0.0007 (7)
O3	0.0123 (7)	0.0216 (7)	0.0083 (7)	0.0009 (6)	0.0011 (6)	−0.0011 (6)
O4	0.0121 (7)	0.0202 (7)	0.0093 (7)	0.0010 (6)	0.0024 (6)	−0.0012 (6)
O5	0.0180 (8)	0.0291 (8)	0.0081 (7)	0.0000 (6)	0.0016 (6)	0.0021 (6)
O6	0.0126 (8)	0.0305 (9)	0.0126 (7)	−0.0007 (7)	−0.0009 (6)	0.0005 (7)
C1	0.0138 (10)	0.0119 (9)	0.0099 (9)	−0.0008 (7)	0.0031 (8)	−0.0019 (8)
C2	0.0134 (10)	0.0103 (9)	0.0130 (10)	0.0020 (8)	0.0032 (8)	0.0014 (8)

Geometric parameters (Å, º) top

Rb1—O2	3.0003 (18)	Co1—O1^viii	2.0690 (16)
Rb1—O5ⁱ	3.0209 (16)	Co1—O1	2.0690 (16)
Rb1—O3ⁱⁱ	3.0819 (15)	Co1—O3^viii	2.0744 (14)
Rb1—O2ⁱⁱⁱ	3.0856 (19)	Co1—O3	2.0744 (14)
Rb1—O5ⁱⁱ	3.1023 (16)	Co1—O4	2.0969 (14)
Rb1—O6^iv	3.1190 (15)	Co1—O4^viii	2.0969 (14)
Rb1—O2^v	3.1461 (19)	O3—C1	1.265 (2)
Rb1—O4^vi	3.1862 (15)	O4—C2	1.276 (3)
Rb1—O1^vii	3.2421 (17)	O5—C1	1.240 (3)
Rb1—O6^v	3.3122 (16)	O6—C2	1.237 (3)
Rb1—O3^vii	3.3497 (15)	C1—C2	1.556 (3)

O2—Rb1—O5ⁱ	62.28 (5)	O2ⁱⁱⁱ—Rb1—O3^vii	58.91 (4)
O2—Rb1—O3ⁱⁱ	62.87 (4)	O5ⁱⁱ—Rb1—O3^vii	149.98 (4)
O5ⁱ—Rb1—O3ⁱⁱ	121.12 (4)	O6^iv—Rb1—O3^vii	69.30 (4)
O2—Rb1—O2ⁱⁱⁱ	105.67 (5)	O2^v—Rb1—O3^vii	116.60 (4)
O5ⁱ—Rb1—O2ⁱⁱⁱ	148.26 (5)	O4^vi—Rb1—O3^vii	58.39 (4)
O3ⁱⁱ—Rb1—O2ⁱⁱⁱ	67.65 (4)	O1^vii—Rb1—O3^vii	52.51 (4)
O2—Rb1—O5ⁱⁱ	65.45 (5)	O6^v—Rb1—O3^vii	84.20 (4)
O5ⁱ—Rb1—O5ⁱⁱ	95.16 (4)	O1^viii—Co1—O1	180.0
O3ⁱⁱ—Rb1—O5ⁱⁱ	42.24 (4)	O1^viii—Co1—O3^viii	89.52 (6)
O2ⁱⁱⁱ—Rb1—O5ⁱⁱ	106.35 (5)	O1—Co1—O3^viii	90.48 (6)
O2—Rb1—O6^iv	72.16 (5)	O1^viii—Co1—O3	90.48 (6)
O5ⁱ—Rb1—O6^iv	90.38 (4)	O1—Co1—O3	89.52 (6)
O3ⁱⁱ—Rb1—O6^iv	92.16 (4)	O3^viii—Co1—O3	180.0
O2ⁱⁱⁱ—Rb1—O6^iv	58.00 (5)	O1^viii—Co1—O4	89.98 (6)
O5ⁱⁱ—Rb1—O6^iv	128.06 (4)	O1—Co1—O4	90.02 (6)
O2—Rb1—O2^v	95.58 (5)	O3^viii—Co1—O4	99.83 (6)
O5ⁱ—Rb1—O2^v	64.67 (5)	O3—Co1—O4	80.17 (6)
O3ⁱⁱ—Rb1—O2^v	101.60 (4)	O1^viii—Co1—O4^viii	90.02 (6)
O2ⁱⁱⁱ—Rb1—O2^v	146.79 (5)	O1—Co1—O4^viii	89.98 (6)
O5ⁱⁱ—Rb1—O2^v	59.77 (4)	O3^viii—Co1—O4^viii	80.17 (6)
O6^iv—Rb1—O2^v	155.02 (4)	O3—Co1—O4^viii	99.83 (6)
O2—Rb1—O4^vi	135.32 (4)	O4—Co1—O4^viii	180.0
O5ⁱ—Rb1—O4^vi	73.17 (4)	Co1—O1—Rb1^vii	91.19 (6)
O3ⁱⁱ—Rb1—O4^vi	151.80 (4)	Rb1—O2—Rb1^ix	95.49 (5)
O2ⁱⁱⁱ—Rb1—O4^vi	114.32 (4)	Rb1—O2—Rb1^v	84.42 (4)
O5ⁱⁱ—Rb1—O4^vi	117.99 (4)	Rb1^ix—O2—Rb1^v	156.77 (7)
O6^iv—Rb1—O4^vi	113.04 (4)	C1—O3—Co1	113.38 (13)
O2^v—Rb1—O4^vi	60.44 (4)	C1—O3—Rb1^x	94.92 (12)
O2—Rb1—O1^vii	101.48 (5)	Co1—O3—Rb1^x	137.42 (6)
O5ⁱ—Rb1—O1^vii	59.06 (4)	C1—O3—Rb1^vii	140.90 (12)
O3ⁱⁱ—Rb1—O1^vii	153.07 (4)	Co1—O3—Rb1^vii	88.13 (5)
O2ⁱⁱⁱ—Rb1—O1^vii	98.78 (5)	Rb1^x—O3—Rb1^vii	88.83 (4)
O5ⁱⁱ—Rb1—O1^vii	153.95 (4)	C2—O4—Co1	112.61 (13)
O6^iv—Rb1—O1^vii	61.33 (4)	C2—O4—Rb1^xi	136.21 (12)
O2^v—Rb1—O1^vii	101.68 (5)	Co1—O4—Rb1^xi	92.24 (5)
O4^vi—Rb1—O1^vii	54.53 (4)	C1—O5—Rb1^xii	141.22 (13)
O2—Rb1—O6^v	126.25 (5)	C1—O5—Rb1^x	94.51 (12)
O5ⁱ—Rb1—O6^v	143.03 (4)	Rb1^xii—O5—Rb1^x	84.84 (4)
O3ⁱⁱ—Rb1—O6^v	66.26 (4)	C2—O6—Rb1^xiii	145.41 (13)
O2ⁱⁱⁱ—Rb1—O6^v	68.49 (4)	C2—O6—Rb1^v	112.75 (13)
O5ⁱⁱ—Rb1—O6^v	65.79 (4)	Rb1^xiii—O6—Rb1^v	88.88 (4)
O6^iv—Rb1—O6^v	126.49 (2)	O5—C1—O3	125.57 (19)
O2^v—Rb1—O6^v	78.39 (4)	O5—C1—C2	118.35 (18)
O4^vi—Rb1—O6^v	87.81 (4)	O3—C1—C2	116.07 (17)
O1^vii—Rb1—O6^v	132.20 (4)	O6—C2—O4	124.8 (2)
O2—Rb1—O3^vii	140.70 (5)	O6—C2—C1	119.63 (18)
O5ⁱ—Rb1—O3^vii	110.22 (4)	O4—C2—C1	115.52 (18)
O3ⁱⁱ—Rb1—O3^vii	125.45 (2)

Symmetry codes: (i) −x+3/2, y+1/2, −z+3/2; (ii) x+1/2, −y+1/2, z−1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) x−1/2, −y+1/2, z−1/2; (v) −x+2, −y+1, −z+1; (vi) x, y+1, z; (vii) −x+1, −y+1, −z+1; (viii) −x+1, −y, −z+1; (ix) −x+3/2, y−1/2, −z+1/2; (x) x−1/2, −y+1/2, z+1/2; (xi) x, y−1, z; (xii) −x+3/2, y−1/2, −z+3/2; (xiii) x+1/2, −y+1/2, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O2—H1···O4	0.89 (4)	2.00 (4)	2.880 (2)	171 (4)
O2—H2···O4^xiv	0.85 (5)	2.47 (5)	3.187 (2)	143 (4)
O2—H2···O6^xiv	0.85 (5)	2.20 (5)	3.008 (2)	159 (4)
O1—H3···O5ⁱ	0.76 (3)	1.98 (3)	2.736 (2)	174 (3)
O1—H4···O6^iv	0.78 (3)	2.05 (3)	2.825 (2)	172 (3)

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

catena-Poly[dirubidium [[dichloridocobalt(II)]-µ-oxalato]] (II) top

Crystal data top

Rb₂[CoCl₂(C₂O₄)]	F(000) = 358
M_r = 388.79	D_x = 2.981 Mg m⁻³
Orthorhombic, Immm	Mo Kα radiation, λ = 0.71075 Å
Hall symbol: -I 2 2	Cell parameters from 800 reflections
a = 5.3445 (3) Å	θ = 3.2–27.5°
b = 6.4380 (4) Å	µ = 13.73 mm⁻¹
c = 12.5866 (8) Å	T = 173 K
V = 433.08 (5) Å³	Prism, purple
Z = 2	0.20 × 0.15 × 0.07 mm

Data collection top

Rigaku Mercury2 (2x2 bin mode) diffractometer	310 independent reflections
Radiation source: Sealed Tube	296 reflections with I > 2σ(I)
Detector resolution: 13.6612 pixels mm^-1	R_int = 0.034
profile data from ω–scans	θ_max = 27.5°, θ_min = 3.2°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −6→6
T_min = 0.671, T_max = 1.00	k = −8→8
2218 measured reflections	l = −16→16

Refinement top

Refinement on F²	22 parameters
Least-squares matrix: full	0 restraints
R[F² > 2σ(F²)] = 0.018	w = 1/[σ²(F_o²) + (0.0276P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.043	(Δ/σ)_max < 0.001
S = 1.11	Δρ_max = 0.63 e Å⁻³
310 reflections	Δρ_min = −0.53 e Å⁻³

Special details top

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

	x	y	z	U_iso*/U_eq
Rb1	0.500000	0.500000	0.34642 (3)	0.01924 (15)
Co1	0.500000	1.000000	0.500000	0.01332 (18)
Cl1	0.500000	1.000000	0.30247 (7)	0.0198 (2)
O1	0.7911 (3)	0.7898 (2)	0.500000	0.0154 (4)
C1	1.000000	0.8775 (5)	0.500000	0.0123 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Rb1	0.0230 (2)	0.0136 (2)	0.0211 (2)	0.000	0.000	0.000
Co1	0.0072 (3)	0.0105 (3)	0.0222 (3)	0.000	0.000	0.000
Cl1	0.0233 (4)	0.0172 (4)	0.0190 (4)	0.000	0.000	0.000
O1	0.0106 (9)	0.0106 (7)	0.0251 (8)	−0.0006 (6)	0.000	0.000
C1	0.0119 (16)	0.0125 (16)	0.0125 (14)	0.000	0.000	0.000

Geometric parameters (Å, º) top

Rb1—O1	3.1045 (13)	Co1—O1^vii	2.0616 (17)
Rb1—O1ⁱ	3.1045 (13)	Co1—O1ⁱ	2.0616 (17)
Rb1—O1ⁱⁱ	3.1045 (13)	Co1—O1^viii	2.0616 (17)
Rb1—O1ⁱⁱⁱ	3.1045 (13)	Co1—O1	2.0616 (17)
Rb1—Cl1^iv	3.2639 (6)	Co1—Cl1^viii	2.4863 (9)
Rb1—Cl1^v	3.2639 (6)	Co1—Cl1	2.4863 (9)
Rb1—Cl1^vi	3.2662 (3)	O1—C1	1.251 (2)
Rb1—Cl1	3.2662 (3)	C1—C1^ix	1.577 (6)

O1—Rb1—O1ⁱ	60.14 (6)	O1^vii—Co1—O1	82.03 (9)
O1—Rb1—O1ⁱⁱ	73.89 (5)	O1ⁱ—Co1—O1	97.97 (9)
O1ⁱ—Rb1—O1ⁱⁱ	102.98 (4)	O1^viii—Co1—O1	180.0
O1—Rb1—O1ⁱⁱⁱ	102.98 (4)	O1^vii—Co1—Cl1^viii	90.0
O1ⁱ—Rb1—O1ⁱⁱⁱ	73.89 (5)	O1ⁱ—Co1—Cl1^viii	90.0
O1ⁱⁱ—Rb1—O1ⁱⁱⁱ	60.14 (6)	O1^viii—Co1—Cl1^viii	90.0
O1—Rb1—Cl1^iv	140.15 (3)	O1—Co1—Cl1^viii	90.0
O1ⁱ—Rb1—Cl1^iv	86.98 (3)	O1^vii—Co1—Cl1	90.0
O1ⁱⁱ—Rb1—Cl1^iv	140.15 (3)	O1ⁱ—Co1—Cl1	90.0
O1ⁱⁱⁱ—Rb1—Cl1^iv	86.98 (3)	O1^viii—Co1—Cl1	90.0
O1—Rb1—Cl1^v	86.98 (3)	O1—Co1—Cl1	90.0
O1ⁱ—Rb1—Cl1^v	140.15 (3)	Cl1^viii—Co1—Cl1	180.0
O1ⁱⁱ—Rb1—Cl1^v	86.98 (3)	Co1—Cl1—Rb1^iv	125.042 (14)
O1ⁱⁱⁱ—Rb1—Cl1^v	140.15 (3)	Co1—Cl1—Rb1^v	125.042 (14)
Cl1^iv—Rb1—Cl1^v	109.92 (3)	Rb1^iv—Cl1—Rb1^v	109.92 (3)
O1—Rb1—Cl1^vi	134.25 (3)	Co1—Cl1—Rb1	80.247 (16)
O1ⁱ—Rb1—Cl1^vi	134.25 (3)	Rb1^iv—Cl1—Rb1	95.582 (8)
O1ⁱⁱ—Rb1—Cl1^vi	60.86 (3)	Rb1^v—Cl1—Rb1	95.582 (8)
O1ⁱⁱⁱ—Rb1—Cl1^vi	60.86 (3)	Co1—Cl1—Rb1^x	80.246 (16)
Cl1^iv—Rb1—Cl1^vi	84.419 (8)	Rb1^iv—Cl1—Rb1^x	95.582 (8)
Cl1^v—Rb1—Cl1^vi	84.419 (8)	Rb1^v—Cl1—Rb1^x	95.582 (8)
O1—Rb1—Cl1	60.86 (3)	Rb1—Cl1—Rb1^x	160.49 (3)
O1ⁱ—Rb1—Cl1	60.86 (3)	C1—O1—Co1	112.18 (16)
O1ⁱⁱ—Rb1—Cl1	134.25 (3)	C1—O1—Rb1ⁱⁱⁱ	135.91 (8)
O1ⁱⁱⁱ—Rb1—Cl1	134.25 (3)	Co1—O1—Rb1ⁱⁱⁱ	90.94 (5)
Cl1^iv—Rb1—Cl1	84.418 (8)	C1—O1—Rb1	135.91 (8)
Cl1^v—Rb1—Cl1	84.418 (8)	Co1—O1—Rb1	90.94 (5)
Cl1^vi—Rb1—Cl1	160.49 (3)	Rb1ⁱⁱⁱ—O1—Rb1	77.02 (4)
O1^vii—Co1—O1ⁱ	180.0	O1^xi—C1—O1	126.4 (3)
O1^vii—Co1—O1^viii	97.97 (9)	O1^xi—C1—C1^ix	116.81 (15)
O1ⁱ—Co1—O1^viii	82.03 (9)	O1—C1—C1^ix	116.81 (15)

Symmetry codes: (i) −x+1, y, −z+1; (ii) x, −y+1, z; (iii) −x+1, −y+1, −z+1; (iv) −x+1/2, −y+3/2, −z+1/2; (v) −x+3/2, −y+3/2, −z+1/2; (vi) x, y−1, z; (vii) x, −y+2, z; (viii) −x+1, −y+2, −z+1; (ix) −x+2, −y+2, −z+1; (x) x, y+1, z; (xi) −x+2, y, −z+1.

Poly[dipotassium [tri-µ-oxalatocopper(II)dilithium] dihydrate] (III) top

Crystal data top

K₂[Li₂Cu(C₂O₄)₃]·2H₂O	Z = 1
M_r = 455.71	F(000) = 225
Triclinic, P1	D_x = 2.310 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71075 Å
a = 6.1847 (4) Å	Cell parameters from 888 reflections
b = 7.2575 (5) Å	θ = 2.5–27.5°
c = 8.1795 (5) Å	µ = 2.38 mm⁻¹
α = 101.327 (11)°	T = 173 K
β = 91.723 (11)°	Prism, blue
γ = 113.563 (11)°	0.14 × 0.14 × 0.07 mm
V = 327.56 (5) Å³

Data collection top

Rigaku Mercury2 (2x2 bin mode) diffractometer	1500 independent reflections
Radiation source: Sealed Tube	1077 reflections with I > 2σ(I)
Detector resolution: 13.6612 pixels mm^-1	R_int = 0.095
profile data from ω–scans	θ_max = 27.5°, θ_min = 2.6°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −8→8
T_min = 0.610, T_max = 1.00	k = −9→9
3403 measured reflections	l = −10→10

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F² > 2σ(F²)] = 0.045	All H-atom parameters refined
wR(F²) = 0.114	w = 1/[σ²(F_o²) + (0.0439P)²] where P = (F_o² + 2F_c²)/3
S = 0.94	(Δ/σ)_max < 0.001
1500 reflections	Δρ_max = 1.03 e Å⁻³
132 parameters	Δρ_min = −1.01 e Å⁻³

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cu1	1.000000	1.000000	1.000000	0.0141 (2)
K1	0.53561 (17)	0.08774 (15)	0.80051 (12)	0.0182 (2)
O1	1.1046 (5)	0.7828 (4)	0.9188 (4)	0.0139 (6)
O2	0.6795 (5)	0.7931 (5)	0.9232 (4)	0.0139 (6)
O3	0.9423 (5)	0.4577 (5)	0.7685 (4)	0.0166 (7)
O4	0.5056 (5)	0.4613 (4)	0.7870 (4)	0.0168 (7)
O5	0.1518 (5)	0.2387 (4)	0.4512 (4)	0.0174 (7)
O6	−0.0303 (6)	−0.0777 (5)	0.2817 (4)	0.0194 (7)
O7A	0.3910 (18)	−0.2142 (15)	0.5335 (14)	0.028 (2)	0.5
O7B	0.3555 (18)	−0.3016 (16)	0.5653 (14)	0.027 (2)	0.5
C1	0.9305 (7)	0.6178 (6)	0.8431 (5)	0.0125 (8)
C2	0.6818 (7)	0.6206 (6)	0.8495 (5)	0.0129 (8)
C3	0.0359 (7)	0.0482 (6)	0.4216 (6)	0.0138 (8)
Li1	0.1867 (13)	0.3767 (13)	0.6931 (10)	0.0205 (17)
H1	0.481 (15)	−0.288 (12)	0.557 (10)	0.06 (3)*
H2	0.283 (15)	−0.343 (13)	0.491 (11)	0.07 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.0105 (4)	0.0100 (4)	0.0191 (4)	0.0037 (3)	0.0009 (3)	−0.0015 (3)
K1	0.0195 (5)	0.0173 (5)	0.0177 (5)	0.0079 (4)	0.0026 (4)	0.0031 (4)
O1	0.0106 (14)	0.0118 (14)	0.0176 (16)	0.0044 (11)	0.0000 (11)	0.0000 (12)
O2	0.0119 (14)	0.0156 (15)	0.0133 (15)	0.0064 (12)	0.0018 (11)	−0.0001 (12)
O3	0.0171 (15)	0.0116 (14)	0.0204 (17)	0.0064 (12)	0.0047 (13)	0.0005 (12)
O4	0.0108 (14)	0.0102 (14)	0.0229 (17)	0.0003 (12)	−0.0022 (12)	−0.0014 (12)
O5	0.0223 (16)	0.0086 (14)	0.0159 (16)	0.0012 (12)	0.0031 (13)	0.0018 (12)
O6	0.0236 (17)	0.0182 (16)	0.0121 (16)	0.0051 (13)	0.0001 (13)	0.0014 (13)
O7A	0.026 (5)	0.012 (4)	0.043 (6)	0.012 (4)	−0.003 (4)	−0.011 (4)
O7B	0.019 (5)	0.014 (5)	0.036 (6)	0.007 (4)	−0.009 (4)	−0.017 (4)
C1	0.014 (2)	0.0117 (19)	0.013 (2)	0.0048 (16)	0.0038 (16)	0.0050 (16)
C2	0.013 (2)	0.016 (2)	0.0092 (19)	0.0061 (17)	0.0011 (15)	0.0027 (16)
C3	0.016 (2)	0.011 (2)	0.017 (2)	0.0089 (17)	0.0019 (17)	0.0034 (17)
Li1	0.010 (3)	0.029 (4)	0.021 (4)	0.010 (3)	0.000 (3)	−0.002 (3)

Geometric parameters (Å, º) top

Cu1—O2	1.938 (3)	O2—C2	1.284 (5)
Cu1—O2ⁱ	1.938 (3)	O3—C1	1.233 (5)
Cu1—O1ⁱ	1.942 (3)	O3—Li1^viii	1.907 (8)
Cu1—O1	1.942 (3)	O4—C2	1.230 (5)
K1—O7A	2.609 (10)	O4—Li1	1.901 (8)
K1—O4	2.814 (3)	O5—C3	1.245 (5)
K1—O2ⁱⁱ	2.821 (3)	O5—Li1	1.997 (9)
K1—O7B	2.854 (10)	O6—C3	1.255 (5)
K1—O1ⁱⁱⁱ	2.878 (3)	O6—Li1^vii	2.049 (9)
K1—O3	2.919 (3)	O7A—H1	0.95 (8)
K1—O2^iv	2.946 (3)	O7A—H2	0.89 (9)
K1—O1^v	3.036 (3)	O7B—H1	0.75 (8)
K1—O7A^vi	3.039 (12)	O7B—H2	0.68 (9)
K1—O6^vii	3.146 (3)	C1—C2	1.549 (6)
K1—O6^vi	3.178 (3)	C3—C3^vii	1.571 (9)
O1—C1	1.271 (5)

O2—Cu1—O2ⁱ	180.0	O1ⁱⁱⁱ—K1—O6^vi	63.34 (8)
O2—Cu1—O1ⁱ	93.40 (12)	O3—K1—O6^vi	58.18 (8)
O2ⁱ—Cu1—O1ⁱ	86.60 (12)	O2^iv—K1—O6^vi	61.26 (8)
O2—Cu1—O1	86.60 (12)	O1^v—K1—O6^vi	131.85 (9)
O2ⁱ—Cu1—O1	93.40 (12)	O7A^vi—K1—O6^vi	75.66 (19)
O1ⁱ—Cu1—O1	180.00 (9)	O6^vii—K1—O6^vi	155.90 (12)
O7A—K1—O4	119.6 (2)	C1—O1—Cu1	110.8 (3)
O7A—K1—O2ⁱⁱ	134.7 (2)	C1—O1—K1ⁱⁱⁱ	137.7 (3)
O4—K1—O2ⁱⁱ	70.35 (9)	Cu1—O1—K1ⁱⁱⁱ	94.37 (11)
O7A—K1—O7B	13.6 (3)	C1—O1—K1^ix	133.0 (3)
O4—K1—O7B	131.3 (3)	Cu1—O1—K1^ix	90.46 (11)
O2ⁱⁱ—K1—O7B	127.0 (2)	K1ⁱⁱⁱ—O1—K1^ix	77.56 (8)
O7A—K1—O1ⁱⁱⁱ	133.6 (2)	C2—O2—Cu1	110.7 (3)
O4—K1—O1ⁱⁱⁱ	101.72 (9)	C2—O2—K1ⁱⁱ	133.6 (3)
O2ⁱⁱ—K1—O1ⁱⁱⁱ	76.43 (9)	Cu1—O2—K1ⁱⁱ	97.23 (11)
O7B—K1—O1ⁱⁱⁱ	125.6 (2)	C2—O2—K1^x	132.4 (3)
O7A—K1—O3	114.9 (3)	Cu1—O2—K1^x	92.37 (11)
O4—K1—O3	56.61 (8)	K1ⁱⁱ—O2—K1^x	79.95 (8)
O2ⁱⁱ—K1—O3	106.84 (9)	C1—O3—Li1^viii	136.6 (4)
O7B—K1—O3	125.5 (2)	C1—O3—K1	112.5 (3)
O1ⁱⁱⁱ—K1—O3	70.04 (9)	Li1^viii—O3—K1	107.9 (3)
O7A—K1—O2^iv	80.2 (2)	C2—O4—Li1	139.7 (4)
O4—K1—O2^iv	159.58 (9)	C2—O4—K1	116.4 (3)
O2ⁱⁱ—K1—O2^iv	100.05 (8)	Li1—O4—K1	103.7 (3)
O7B—K1—O2^iv	69.0 (2)	C3—O5—Li1	113.3 (4)
O1ⁱⁱⁱ—K1—O2^iv	57.99 (8)	C3—O6—Li1^vii	111.7 (4)
O3—K1—O2^iv	112.41 (9)	C3—O6—K1^vii	100.4 (3)
O7A—K1—O1^v	80.5 (3)	Li1^vii—O6—K1^vii	89.8 (2)
O4—K1—O1^v	113.85 (9)	C3—O6—K1^vi	99.4 (3)
O2ⁱⁱ—K1—O1^v	57.50 (8)	Li1^vii—O6—K1^vi	95.6 (2)
O7B—K1—O1^v	70.1 (2)	K1^vii—O6—K1^vi	155.90 (12)
O1ⁱⁱⁱ—K1—O1^v	102.44 (8)	K1—O7A—K1^vi	115.8 (4)
O3—K1—O1^v	164.28 (9)	K1—O7A—H1	100 (5)
O2^iv—K1—O1^v	72.19 (8)	K1^vi—O7A—H1	113 (5)
O7A—K1—O7A^vi	64.2 (4)	K1—O7A—H2	144 (6)
O4—K1—O7A^vi	64.04 (18)	K1^vi—O7A—H2	96 (6)
O2ⁱⁱ—K1—O7A^vi	132.00 (18)	H1—O7A—H2	81 (7)
O7B—K1—O7A^vi	77.7 (4)	K1—O7B—H1	89 (6)
O1ⁱⁱⁱ—K1—O7A^vi	126.0 (2)	K1—O7B—H2	135 (8)
O3—K1—O7A^vi	58.7 (2)	H1—O7B—H2	113 (9)
O2^iv—K1—O7A^vi	127.94 (18)	O3—C1—O1	126.1 (4)
O1^v—K1—O7A^vi	131.4 (2)	O3—C1—C2	118.0 (4)
O7A—K1—O6^vii	82.2 (2)	O1—C1—C2	115.9 (4)
O4—K1—O6^vii	61.81 (9)	O4—C2—O2	125.6 (4)
O2ⁱⁱ—K1—O6^vii	63.59 (8)	O4—C2—C1	118.7 (4)
O7B—K1—O6^vii	84.8 (2)	O2—C2—C1	115.7 (3)
O1ⁱⁱⁱ—K1—O6^vii	139.77 (9)	O5—C3—O6	128.1 (4)
O3—K1—O6^vii	116.35 (9)	O5—C3—C3^vii	116.4 (5)
O2^iv—K1—O6^vii	131.16 (9)	O6—C3—C3^vii	115.6 (5)
O1^v—K1—O6^vii	60.12 (8)	O4—Li1—O3^xi	131.6 (5)
O7A^vi—K1—O6^vii	81.9 (2)	O4—Li1—O5	108.5 (4)
O7A—K1—O6^vi	80.2 (2)	O3^xi—Li1—O5	117.8 (4)
O4—K1—O6^vi	114.08 (9)	O4—Li1—O6^vii	102.2 (4)
O2ⁱⁱ—K1—O6^vi	139.69 (9)	O3^xi—Li1—O6^vii	97.4 (4)
O7B—K1—O6^vi	82.0 (2)	O5—Li1—O6^vii	82.4 (3)

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

Cu—O bond Lengths of Compound III top

Bond	Bond distance (Å)
Cu—O1	1.942 (3)
Cu—O1ⁱ	1.942 (3)
Cu—O2	1.938 (3)
Cu—O2ⁱ	1.938 (3)
Cu—O6	2.473 (4)
Cu—O6ⁱ	2.473 (4)

Symmetry codes: (i) -x + 2, -y + 2, -z + 2.

Funding information

The authors would like to acknowledge the EPSRC for a Doctoral studentship to RC DTG012 EP/K503162–1 and the Swedish foundation for strategic research (SSF), project contract EM-16–0039.

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Volume 79| Part 4| April 2023| Pages 267-271

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