{[Na1(μ-H2O)Na2]2[(C2O4)2Cr(μ-OH)2Cr(C2O4)2]·H2O}n, a novel hydrated form

Bélombé, M.M.; Nenwa, J.; Ngouné, J.; Álvarez, E.; Galindo, A.

doi:10.1107/S1600536810023986

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 8| August 2010| Pages m990-m991

https://doi.org/10.1107/S1600536810023986

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{[Na1(μ-H₂O)Na2]₂[(C₂O₄)₂Cr(μ-OH)₂Cr(C₂O₄)₂]·H₂O}_n, a novel hydrated form

Michel M. Bélombé,^a Justin Nenwa,^a Jean Ngouné,^b Eleuterio Álvarez ^c ^* and Agustín Galindo ^d

^aDepartment of Inorganic Chemistry, Faculty of Science, POB 812, University of Yaounde I, Cameroon, ^bDepartment of Chemistry, Faculty of Science, University of Dschang, POB 67, Dschang, Cameroon, ^cInstituto de Investigaciones Químicas, CSIC, Universidad de Sevilla, Avda. Américo Vespucio 49, 41092 Sevilla, Spain, and ^dDepartamento de Química Inorgánica, Universidad de Sevilla, Aptdo 1203, 41071 Sevilla, Spain
^*Correspondence e-mail: ealvarez@iiq.csic.es

(Received 3 May 2010; accepted 21 June 2010; online 21 July 2010)

The unit cell of the title compound, poly[[μ-aqua-μ-hydroxido-di-μ-oxalato-chromium(III)disodium] monohydrate], {[CrNa₂(C₂O₄)₂(OH)(H₂O)]·H₂O}_n, contains four [Na1(μ-H₂O)Na2][(C₂O₄)₂Cr(μ-OH)·H₂O] formula units, each of which consists of two crystallographically independent Na⁺ sites (bridged by one aqua ligand), one half of a centrosymmetric di-μ-hydroxido-bis[cis-bis(oxalato)chromate(III)] dimer, [(C₂O₄)₂Cr(μ-OH)₂Cr(C₂O₄)₂]⁴⁻, and one uncoordinated water molecule. The structure is best described as a coordination polymer in which the three-dimensional lattice framework is realized by the interconnection of the metallic atoms via the O atoms of the aqua, hydroxide and oxalate ligands. One Na atom is heptacoordinated by one water, one hydroxide and five oxalate O atoms, whilst the other is pentacoordinated by one water and four oxalate O atoms. The coordination around the Cr³⁺ sites is pseudo-octahedral, involving four aqua and two hydroxide O atoms. Adjacent Na atoms are separated by 3.593 (2) Å, whereas the intradimer Cr⋯Cr spacing is 2.978 (1) Å. The crystal structure is consolidated by extended relatively weak O—H⋯O hydrogen bonding with O⋯O distances ranging from 2.808 (4) to 3.276 (5) Å.

Related literature

For general background, see: Ferreira et al. (2001 ); Köse et al. (2009 ). For a related structure with a different number of water molecules, see: Scaringe et al. (1977 ).

Experimental

Crystal data

[CrNa₂(C₂O₄)₂(OH)(H₂O)]·H₂O
M_r = 327.06
Monoclinic, P 2₁ /c
a = 9.4776 (10) Å
b = 8.603 (1) Å
c = 12.5353 (14) Å
β = 102.503 (2)°
V = 997.84 (19) Å³
Z = 4
Mo Kα radiation
μ = 1.29 mm⁻¹
T = 173 K
0.60 × 0.12 × 0.10 mm

Data collection

Bruker–Nonius X8 Kappa APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker 2005 ) T_min = 0.832, T_max = 0.882
13658 measured reflections
2018 independent reflections
1625 reflections with I > 2σ(I)
R_int = 0.037

Refinement

R[F² > 2σ(F²)] = 0.044
wR(F²) = 0.133
S = 1.14
2018 reflections
175 parameters
6 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.85 e Å⁻³
Δρ_min = −0.80 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O11—H11B⋯O9ⁱ	0.88 (2)	2.23 (2)	3.080 (5)	163 (5)
O11—H11A⋯O6	0.88 (4)	2.53 (4)	3.144 (5)	128 (4)
O11—H11A⋯O3	0.88 (4)	2.25 (4)	2.949 (4)	137 (4)
O10—H10B⋯O5ⁱⁱ	0.88 (4)	2.36 (4)	3.123 (4)	144 (5)
O10—H10A⋯O5ⁱⁱⁱ	0.91 (2)	2.02 (2)	2.922 (5)	179 (4)
O1—H1⋯O11^iv	0.85	2.01	2.808 (4)	156
Symmetry codes: (i) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) x-1, y, z; (iii) -x+1, -y+1, -z+1; (iv) $[x, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT; program(s) used to solve structure: SIR2002 (Burla et al., 2003 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810023986/pb2030sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810023986/pb2030Isup2.hkl

checkCIF report

Comment top

Scaringe et al. (1977) have previously studied the system Na₄[Cr(ox)₂OH]₂.6H₂O (ox = C₂O₄^2-), paying special attention to its structural-magnetic correlations. We report herein compound (I) as a novel hydrated form of this system, which involves a different number of water molecules and exhibits a different mode of coordinative polymerization.

Fig. 1 depicts the centrosymmetric anionic dimer, [(C₂O₄)₂Cr(µ-OH)₂Cr(C₂O₄)₂]^4-, which constitutes the main structural motif of (I). It is virtually identical to the motif reported previously (Scaringe et al.,1977), as revealed by the closely comparable geometric parameters (Table 1). A larger portion of the structure of (I) is shown in Fig. 2, highlighting heptacoordination of Na1, pentacoordination of Na2 by O atoms, and the bridging of these metallic sites by an aqua ligand (O10). The oxygen atom, O11, is seen to be part of a water molecule of crystallization.

Beyond their identical P2₁/c space group, the two structures present a number of differing features. The crystal data of (I) compare with the reported values (in square brackets) as follows: a = 9.478 (1) [19.530 (12)] Å; b = 8.603 (1) [9.860 (7)] Å; c = 12.535 (1) [12.657 (10)] Å; β = 102.50 [106.93]°; R_final = 4.4 [6.1] %; Z = 4 [4]; D_x = 2.177 [1.966] Mgm^3-; T(K) = 173 [293]. The asymmetric unit of the reported structure contains six H₂O molecules and four crystallographically independent Na⁺ sites, whereby Na1 and Na3 are bridged by the aqua oxygen atom, WO(2), and Na2 and Na4 by the aqua oxygen atom, WO(1), with each Na⁺ site assuming coordination number 6. The asymmetric unit of (I), by contrast, contains four Na⁺ ions (located at two crystallographically independent sites) and four H₂O molecules. Note, furthermore, that coordination numbers 5 and 6 by O atoms have been frequently reported in the literature (Scaringe et al., 1977; Ferreira et al., 2001; Köse et al., 2009), but coordination number 7, if any, is rather scarce for Na⁺. Like in the reported material, the bulk structure of (I) is consolidated by O—H···O bridgings which are, however, stronger in the former than in the latter case (Table 2).

Preliminary observations from our laboratory promisingly suggest that a well conceived and systematically conducted preparative procedure may be applied generally to fabricate a whole range of homologous magnetic materials, provided appropriate paramagnetic transition metal centers are involved.

Related literature top

For general background [to what?], see: Ferreira et al. (2001); Köse et al. (2009). For a related structure, see: Scaringe et al. (1977).

Experimental top

Go In an initial attempt to prepare the targeted material of empirical formula [Ba₂(H₂O)₆][Cr₂(OH)₂(C₂O₄)₄].H₂O, compound (I), instead, was obtained as follows: Cr(NO₃)₃.9H₂O (4.0 g, 10 mmol, Riedel-de Haën, pure) was dissolved at room temperature in H₂O (150 ml) and filtered. H₂C₂O₄.2H₂O (2.6 g, 20 mmol, Riedel-de Haën, 99.5–100.5%) was dissolved therein. This solution was added dropwise to a suspension of Na₂CO₃ (1.6 g, 15 mmol, Riedel-de Haën, 99%) and Ba(OH)₂.8H₂O (3.2 g, 10 mmol, Merck, p.a.) in 200 ml of water, and stirred overnight at ca 70 °C. The violet mass that had formed was filtered off, washed twice with 15 ml H₂O and dried between filter papers. A second crop of material was obtained by concentrating the mother liquor to a volume of ca 20 ml, washing the material twice with 5 ml H₂O and drying it as above. Recrystallization from oversaturated aqueous solution yielded prismatic violet crystals appropriate for X-ray diffractions.

Structure description top

For general background [to what?], see: Ferreira et al. (2001); Köse et al. (2009). For a related structure, see: Scaringe et al. (1977).

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SIR2002 (Burla et al., 2003); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. ORTEP drawing of the anionic dimer, [(C₂O₄)₂Cr(µ-OH)₂Cr(C₂O₄)₂]^4-, in the title compound with atom labeling and numbering. Displacement ellipsoids are drawn at the 50% probability level.
	Fig. 2. Larger portion of the structure of (I) projected onto the (-110) crystallographic plane, highlighting the nonmolecular coordinative polymerization

Poly[[µ-aqua-µ-hydroxido-di-µ-oxalato-chromium(III)disodium] monohydrate] top

Crystal data top

[CrNa₂(C₂O₄)₂(OH)(H₂O)]·H₂O	F(000) = 652
M_r = 327.06	D_x = 2.177 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 6874 reflections
a = 9.4776 (10) Å	θ = 2.2–26.1°
b = 8.603 (1) Å	µ = 1.29 mm⁻¹
c = 12.5353 (14) Å	T = 173 K
β = 102.503 (2)°	Prism, violet
V = 997.84 (19) Å³	0.60 × 0.12 × 0.10 mm
Z = 4

Data collection top

Bruker–Nonius X8 Kappa APEXII CCD area-detector diffractometer	2018 independent reflections
Radiation source: fine-focus sealed tube	1625 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.037
Detector resolution: 8.26 pixels mm^-1	θ_max = 26.4°, θ_min = 2.2°
phi and ω scans with narrow frames	h = −11→11
Absorption correction: multi-scan (APEX2; Bruker 2005)	k = −10→10
T_min = 0.832, T_max = 0.882	l = −15→15
13658 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.044	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.133	H atoms treated by a mixture of independent and constrained refinement
S = 1.14	w = 1/[σ²(F_o²) + (0.054P)² + 4.054P] where P = (F_o² + 2F_c²)/3
2018 reflections	(Δ/σ)_max < 0.001
175 parameters	Δρ_max = 0.85 e Å⁻³
6 restraints	Δρ_min = −0.80 e Å⁻³

Crystal data top

[CrNa₂(C₂O₄)₂(OH)(H₂O)]·H₂O	V = 997.84 (19) Å³
M_r = 327.06	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 9.4776 (10) Å	µ = 1.29 mm⁻¹
b = 8.603 (1) Å	T = 173 K
c = 12.5353 (14) Å	0.60 × 0.12 × 0.10 mm
β = 102.503 (2)°

Data collection top

Bruker–Nonius X8 Kappa APEXII CCD area-detector diffractometer	2018 independent reflections
Absorption correction: multi-scan (APEX2; Bruker 2005)	1625 reflections with I > 2σ(I)
T_min = 0.832, T_max = 0.882	R_int = 0.037
13658 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.044	6 restraints
wR(F²) = 0.133	H atoms treated by a mixture of independent and constrained refinement
S = 1.14	Δρ_max = 0.85 e Å⁻³
2018 reflections	Δρ_min = −0.80 e Å⁻³
175 parameters

Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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 > σ(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 (Å²) top

	x	y	z	U_iso*/U_eq
Cr1	0.60366 (7)	0.06037 (8)	0.43610 (5)	0.0210 (2)
Na1	0.36188 (17)	0.3337 (2)	0.48733 (13)	0.0265 (4)
Na2	0.14538 (19)	0.3470 (2)	0.21413 (15)	0.0327 (4)
O1	0.5272 (3)	0.1171 (4)	0.5646 (2)	0.0237 (6)
H1	0.5819	0.1507	0.6229	0.028*
O2	0.7636 (3)	−0.0653 (3)	0.5189 (2)	0.0231 (6)
O3	0.7506 (3)	0.2268 (4)	0.4659 (2)	0.0249 (6)
O4	0.9836 (3)	−0.0410 (4)	0.6268 (2)	0.0298 (7)
O5	0.9674 (3)	0.2755 (4)	0.5739 (3)	0.0313 (7)
O6	0.6501 (3)	0.0117 (4)	0.2928 (2)	0.0249 (6)
O7	0.4467 (3)	0.1816 (4)	0.3427 (2)	0.0242 (6)
O8	0.5513 (3)	0.0306 (4)	0.1139 (2)	0.0281 (7)
O9	0.3141 (3)	0.1684 (4)	0.1719 (2)	0.0277 (7)
C1	0.8758 (4)	0.0129 (5)	0.5650 (3)	0.0241 (9)
C2	0.8674 (4)	0.1875 (6)	0.5347 (3)	0.0256 (9)
C3	0.4236 (4)	0.1425 (5)	0.2411 (3)	0.0230 (8)
C4	0.5518 (4)	0.0536 (5)	0.2099 (3)	0.0222 (8)
O10	0.1206 (3)	0.4049 (4)	0.3955 (3)	0.0344 (8)
H10A	0.094 (5)	0.504 (2)	0.405 (5)	0.051*
H10B	0.058 (5)	0.345 (4)	0.419 (4)	0.051*
O11	0.7568 (4)	0.3460 (4)	0.2464 (3)	0.0370 (8)
H11A	0.777 (6)	0.271 (4)	0.295 (3)	0.055*
H11B	0.756 (6)	0.438 (3)	0.277 (4)	0.055*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cr1	0.0155 (3)	0.0329 (4)	0.0148 (3)	0.0002 (3)	0.0036 (2)	0.0002 (3)
Na1	0.0221 (8)	0.0386 (10)	0.0185 (8)	0.0001 (7)	0.0035 (6)	0.0001 (7)
Na2	0.0212 (9)	0.0438 (11)	0.0309 (9)	0.0028 (8)	0.0005 (7)	−0.0031 (8)
O1	0.0202 (14)	0.0366 (17)	0.0142 (13)	−0.0032 (13)	0.0033 (10)	−0.0020 (12)
O2	0.0176 (13)	0.0314 (16)	0.0195 (14)	−0.0025 (12)	0.0022 (11)	−0.0005 (12)
O3	0.0201 (14)	0.0319 (16)	0.0220 (14)	−0.0023 (12)	0.0031 (11)	0.0025 (12)
O4	0.0205 (14)	0.0414 (19)	0.0256 (15)	0.0007 (13)	0.0006 (12)	0.0036 (14)
O5	0.0218 (15)	0.0393 (18)	0.0310 (16)	−0.0061 (14)	0.0015 (13)	0.0006 (14)
O6	0.0194 (14)	0.0391 (18)	0.0168 (13)	0.0036 (13)	0.0050 (11)	0.0013 (12)
O7	0.0216 (14)	0.0355 (17)	0.0163 (13)	0.0012 (12)	0.0060 (11)	−0.0006 (12)
O8	0.0287 (16)	0.0378 (18)	0.0178 (14)	0.0059 (13)	0.0054 (12)	−0.0004 (13)
O9	0.0215 (14)	0.0433 (19)	0.0169 (14)	0.0033 (13)	0.0012 (11)	0.0011 (13)
C1	0.021 (2)	0.038 (2)	0.0150 (18)	0.0019 (18)	0.0076 (16)	−0.0012 (17)
C2	0.0187 (19)	0.042 (3)	0.0176 (19)	0.0016 (18)	0.0066 (15)	−0.0012 (18)
C3	0.022 (2)	0.028 (2)	0.0195 (19)	−0.0008 (17)	0.0059 (15)	−0.0004 (17)
C4	0.0182 (18)	0.028 (2)	0.0199 (19)	0.0029 (17)	0.0043 (15)	0.0018 (16)
O10	0.0274 (17)	0.042 (2)	0.0349 (17)	−0.0011 (15)	0.0096 (14)	0.0058 (16)
O11	0.0386 (19)	0.046 (2)	0.0235 (16)	−0.0009 (17)	0.0009 (14)	0.0064 (15)

Geometric parameters (Å, º) top

Cr1—O2	1.965 (3)	O2—C1	1.286 (5)
Cr1—O1	1.965 (3)	O2—Na1ⁱ	2.591 (3)
Cr1—O1ⁱ	1.966 (3)	O3—C2	1.292 (5)
Cr1—O3	1.976 (3)	O4—C1	1.231 (5)
Cr1—O7	1.979 (3)	O4—Na2^v	2.368 (4)
Cr1—O6	1.985 (3)	O5—C2	1.230 (5)
Cr1—Cr1ⁱ	2.9781 (13)	O5—Na2^v	2.400 (4)
Na1—O8ⁱⁱ	2.368 (3)	O6—C4	1.288 (5)
Na1—O10	2.406 (4)	O6—Na2^vi	2.418 (3)
Na1—O8ⁱⁱⁱ	2.423 (3)	O7—C3	1.289 (5)
Na1—O9ⁱⁱⁱ	2.452 (3)	O8—C4	1.219 (5)
Na1—O1	2.492 (3)	O8—Na1^vi	2.368 (3)
Na1—O7	2.505 (3)	O8—Na1^vii	2.423 (3)
Na1—O2ⁱ	2.591 (3)	O9—C3	1.220 (5)
Na1—C3ⁱⁱⁱ	3.114 (4)	O9—Na1^vii	2.452 (3)
Na1—C4ⁱⁱⁱ	3.129 (4)	C1—C2	1.547 (7)
Na2—O9	2.359 (4)	C1—Na2^v	3.067 (5)
Na2—O4^iv	2.368 (4)	C2—Na2^v	3.086 (4)
Na2—O10	2.389 (4)	C3—C4	1.556 (6)
Na2—O5^iv	2.400 (4)	C3—Na1^vii	3.114 (4)
Na2—O6ⁱⁱ	2.418 (3)	C4—Na1^vii	3.129 (4)
Na2—C1^iv	3.067 (5)	O10—H10A	0.905 (19)
Na2—C2^iv	3.086 (4)	O10—H10B	0.88 (4)
Na2—C3	3.127 (5)	O11—H11A	0.88 (4)
O1—Cr1ⁱ	1.966 (3)	O11—H11B	0.879 (19)
O1—H1	0.8500

O2—Cr1—O1	94.76 (12)	O9—Na2—O4^iv	139.26 (13)
O2—Cr1—O1ⁱ	89.36 (12)	O9—Na2—O10	124.12 (13)
O1—Cr1—O1ⁱ	81.50 (13)	O4^iv—Na2—O10	96.07 (13)
O2—Cr1—O3	82.37 (12)	O9—Na2—O5^iv	87.29 (12)
O1—Cr1—O3	92.00 (12)	O4^iv—Na2—O5^iv	71.87 (12)
O1ⁱ—Cr1—O3	169.05 (12)	O10—Na2—O5^iv	126.18 (13)
O2—Cr1—O7	175.76 (12)	O9—Na2—O6ⁱⁱ	77.65 (12)
O1—Cr1—O7	89.46 (12)	O4^iv—Na2—O6ⁱⁱ	90.80 (12)
O1ⁱ—Cr1—O7	90.79 (12)	O10—Na2—O6ⁱⁱ	99.01 (12)
O3—Cr1—O7	97.99 (13)	O5^iv—Na2—O6ⁱⁱ	132.29 (13)
O2—Cr1—O6	93.73 (12)	O9—Na2—C1^iv	129.40 (12)
O1—Cr1—O6	170.95 (12)	O4^iv—Na2—C1^iv	21.68 (12)
O1ⁱ—Cr1—O6	95.49 (12)	O10—Na2—C1^iv	104.93 (13)
O3—Cr1—O6	92.21 (13)	O5^iv—Na2—C1^iv	50.62 (12)
O7—Cr1—O6	82.03 (12)	O6ⁱⁱ—Na2—C1^iv	108.42 (13)
O2—Cr1—Cr1ⁱ	92.71 (9)	O9—Na2—C2^iv	106.68 (12)
O1—Cr1—Cr1ⁱ	40.76 (9)	O4^iv—Na2—C2^iv	50.63 (12)
O1ⁱ—Cr1—Cr1ⁱ	40.74 (8)	O10—Na2—C2^iv	118.00 (13)
O3—Cr1—Cr1ⁱ	132.15 (9)	O5^iv—Na2—C2^iv	21.61 (12)
O7—Cr1—Cr1ⁱ	90.16 (9)	O6ⁱⁱ—Na2—C2^iv	126.49 (13)
O6—Cr1—Cr1ⁱ	135.64 (10)	C1^iv—Na2—C2^iv	29.13 (12)
O2—Cr1—Na1	138.28 (9)	O9—Na2—C3	20.12 (10)
O1—Cr1—Na1	45.45 (9)	O4^iv—Na2—C3	153.25 (13)
O1ⁱ—Cr1—Na1	94.96 (9)	O10—Na2—C3	105.60 (12)
O3—Cr1—Na1	86.57 (9)	O5^iv—Na2—C3	105.94 (12)
O7—Cr1—Na1	45.92 (9)	O6ⁱⁱ—Na2—C3	70.73 (12)
O6—Cr1—Na1	126.90 (9)	C1^iv—Na2—C3	149.17 (12)
Cr1ⁱ—Cr1—Na1	66.06 (4)	C2^iv—Na2—C3	126.28 (13)
O2—Cr1—Na1ⁱ	46.42 (9)	O9—Na2—Na1	85.31 (9)
O1—Cr1—Na1ⁱ	92.56 (10)	O4^iv—Na2—Na1	129.94 (10)
O1ⁱ—Cr1—Na1ⁱ	43.47 (9)	O10—Na2—Na1	41.66 (9)
O3—Cr1—Na1ⁱ	128.78 (9)	O5^iv—Na2—Na1	148.19 (11)
O7—Cr1—Na1ⁱ	133.03 (9)	O6ⁱⁱ—Na2—Na1	75.87 (8)
O6—Cr1—Na1ⁱ	91.04 (10)	C1^iv—Na2—Na1	145.29 (10)
Cr1ⁱ—Cr1—Na1ⁱ	63.28 (4)	C2^iv—Na2—Na1	155.93 (10)
Na1—Cr1—Na1ⁱ	129.34 (3)	C3—Na2—Na1	65.47 (8)
O8ⁱⁱ—Na1—O10	88.06 (12)	O9—Na2—Na1^vii	31.00 (8)
O8ⁱⁱ—Na1—O8ⁱⁱⁱ	73.25 (12)	O4^iv—Na2—Na1^vii	108.28 (10)
O10—Na1—O8ⁱⁱⁱ	133.10 (14)	O10—Na2—Na1^vii	153.53 (10)
O8ⁱⁱ—Na1—O9ⁱⁱⁱ	131.85 (13)	O5^iv—Na2—Na1^vii	72.98 (9)
O10—Na1—O9ⁱⁱⁱ	95.89 (12)	O6ⁱⁱ—Na2—Na1^vii	71.10 (9)
O8ⁱⁱⁱ—Na1—O9ⁱⁱⁱ	69.37 (11)	C1^iv—Na2—Na1^vii	101.51 (9)
O8ⁱⁱ—Na1—O1	118.75 (12)	C2^iv—Na2—Na1^vii	86.29 (9)
O10—Na1—O1	145.98 (14)	C3—Na2—Na1^vii	48.18 (8)
O8ⁱⁱⁱ—Na1—O1	77.96 (11)	Na1—Na2—Na1^vii	112.08 (6)
O9ⁱⁱⁱ—Na1—O1	81.77 (11)	Cr1—O1—Cr1ⁱ	98.50 (13)
O8ⁱⁱ—Na1—O7	77.46 (11)	Cr1—O1—Na1	100.35 (12)
O10—Na1—O7	101.98 (12)	Cr1ⁱ—O1—Na1	103.65 (12)
O8ⁱⁱⁱ—Na1—O7	114.66 (12)	Cr1—O1—H1	121.6
O9ⁱⁱⁱ—Na1—O7	146.39 (13)	Cr1ⁱ—O1—H1	122.4
O1—Na1—O7	67.50 (10)	Na1—O1—H1	107.1
O8ⁱⁱ—Na1—O2ⁱ	146.29 (12)	C1—O2—Cr1	114.7 (3)
O10—Na1—O2ⁱ	80.21 (12)	C1—O2—Na1ⁱ	144.1 (3)
O8ⁱⁱⁱ—Na1—O2ⁱ	136.02 (12)	Cr1—O2—Na1ⁱ	100.25 (12)
O9ⁱⁱⁱ—Na1—O2ⁱ	81.06 (11)	C2—O3—Cr1	113.8 (3)
O1—Na1—O2ⁱ	65.86 (10)	C1—O4—Na2^v	113.0 (3)
O7—Na1—O2ⁱ	74.32 (10)	C2—O5—Na2^v	112.4 (3)
O8ⁱⁱ—Na1—C3ⁱⁱⁱ	119.34 (12)	C4—O6—Cr1	114.1 (2)
O10—Na1—C3ⁱⁱⁱ	114.87 (12)	C4—O6—Na2^vi	125.5 (2)
O8ⁱⁱⁱ—Na1—C3ⁱⁱⁱ	49.52 (11)	Cr1—O6—Na2^vi	119.51 (13)
O9ⁱⁱⁱ—Na1—C3ⁱⁱⁱ	21.37 (10)	C3—O7—Cr1	113.1 (3)
O1—Na1—C3ⁱⁱⁱ	71.88 (11)	C3—O7—Na1	147.0 (3)
O7—Na1—C3ⁱⁱⁱ	139.02 (12)	Cr1—O7—Na1	99.50 (11)
O2ⁱ—Na1—C3ⁱⁱⁱ	94.18 (11)	C4—O8—Na1^vi	135.9 (3)
O8ⁱⁱ—Na1—C4ⁱⁱⁱ	93.25 (12)	C4—O8—Na1^vii	114.3 (3)
O10—Na1—C4ⁱⁱⁱ	130.64 (13)	Na1^vi—O8—Na1^vii	106.75 (12)
O8ⁱⁱⁱ—Na1—C4ⁱⁱⁱ	20.80 (10)	C3—O9—Na2	118.2 (3)
O9ⁱⁱⁱ—Na1—C4ⁱⁱⁱ	49.37 (10)	C3—O9—Na1^vii	111.6 (3)
O1—Na1—C4ⁱⁱⁱ	72.13 (11)	Na2—O9—Na1^vii	119.28 (14)
O7—Na1—C4ⁱⁱⁱ	126.47 (11)	O4—C1—O2	125.4 (4)
O2ⁱ—Na1—C4ⁱⁱⁱ	118.33 (11)	O4—C1—C2	120.8 (4)
C3ⁱⁱⁱ—Na1—C4ⁱⁱⁱ	28.86 (10)	O2—C1—C2	113.8 (3)
O8ⁱⁱ—Na1—Cr1	93.80 (9)	O4—C1—Na2^v	45.3 (2)
O10—Na1—Cr1	133.43 (11)	O2—C1—Na2^v	168.2 (3)
O8ⁱⁱⁱ—Na1—Cr1	91.29 (9)	C2—C1—Na2^v	76.1 (2)
O9ⁱⁱⁱ—Na1—Cr1	115.97 (10)	O5—C2—O3	125.5 (4)
O1—Na1—Cr1	34.20 (7)	O5—C2—C1	120.3 (4)
O7—Na1—Cr1	34.58 (7)	O3—C2—C1	114.1 (4)
O2ⁱ—Na1—Cr1	72.85 (8)	O5—C2—Na2^v	46.0 (2)
C3ⁱⁱⁱ—Na1—Cr1	104.50 (9)	O3—C2—Na2^v	169.9 (3)
C4ⁱⁱⁱ—Na1—Cr1	95.76 (9)	C1—C2—Na2^v	74.8 (2)
O8ⁱⁱ—Na1—Cr1ⁱ	144.36 (10)	O9—C3—O7	126.2 (4)
O10—Na1—Cr1ⁱ	113.46 (10)	O9—C3—C4	120.1 (4)
O8ⁱⁱⁱ—Na1—Cr1ⁱ	105.90 (9)	O7—C3—C4	113.7 (3)
O9ⁱⁱⁱ—Na1—Cr1ⁱ	76.17 (9)	O9—C3—Na1^vii	47.1 (2)
O1—Na1—Cr1ⁱ	32.88 (7)	O7—C3—Na1^vii	161.1 (3)
O7—Na1—Cr1ⁱ	70.66 (8)	C4—C3—Na1^vii	76.1 (2)
O2ⁱ—Na1—Cr1ⁱ	33.33 (7)	O7—C3—Na2	85.3 (2)
C3ⁱⁱⁱ—Na1—Cr1ⁱ	78.41 (9)	C4—C3—Na2	159.3 (3)
C4ⁱⁱⁱ—Na1—Cr1ⁱ	93.08 (9)	Na1^vii—C3—Na2	83.39 (11)
Cr1—Na1—Cr1ⁱ	50.66 (3)	O8—C4—O6	126.7 (4)
O8ⁱⁱ—Na1—Na2	70.09 (9)	O8—C4—C3	119.5 (4)
O10—Na1—Na2	41.28 (9)	O6—C4—C3	113.8 (3)
O8ⁱⁱⁱ—Na1—Na2	142.94 (10)	O6—C4—Na1^vii	169.2 (3)
O9ⁱⁱⁱ—Na1—Na2	135.70 (9)	C3—C4—Na1^vii	75.1 (2)
O1—Na1—Na2	125.14 (9)	Na2—O10—Na1	97.06 (13)
O7—Na1—Na2	62.18 (8)	Na2—O10—H10A	114 (3)
O2ⁱ—Na1—Na2	80.56 (8)	Na1—O10—H10A	116 (4)
C3ⁱⁱⁱ—Na1—Na2	156.03 (10)	Na2—O10—H10B	114 (3)
C4ⁱⁱⁱ—Na1—Na2	160.00 (10)	Na1—O10—H10B	109 (3)
Cr1—Na1—Na2	96.31 (5)	H10A—O10—H10B	106 (3)
Cr1ⁱ—Na1—Na2	106.90 (6)	H11A—O11—H11B	112 (3)

O2—Cr1—Na1—O8ⁱⁱ	117.77 (15)	O8ⁱⁱ—Na1—O1—Cr1ⁱ	−149.18 (12)
O1—Cr1—Na1—O8ⁱⁱ	139.46 (15)	O10—Na1—O1—Cr1ⁱ	−11.1 (3)
O1ⁱ—Cr1—Na1—O8ⁱⁱ	−147.61 (12)	O8ⁱⁱⁱ—Na1—O1—Cr1ⁱ	147.75 (13)
O3—Cr1—Na1—O8ⁱⁱ	43.26 (12)	O9ⁱⁱⁱ—Na1—O1—Cr1ⁱ	77.21 (12)
O7—Cr1—Na1—O8ⁱⁱ	−61.33 (14)	O7—Na1—O1—Cr1ⁱ	−88.88 (13)
O6—Cr1—Na1—O8ⁱⁱ	−46.93 (15)	O2ⁱ—Na1—O1—Cr1ⁱ	−6.63 (10)
Cr1ⁱ—Cr1—Na1—O8ⁱⁱ	−177.08 (9)	C3ⁱⁱⁱ—Na1—O1—Cr1ⁱ	96.70 (13)
Na1ⁱ—Cr1—Na1—O8ⁱⁱ	−177.08 (9)	C4ⁱⁱⁱ—Na1—O1—Cr1ⁱ	127.07 (13)
O2—Cr1—Na1—O10	−151.31 (18)	Cr1—Na1—O1—Cr1ⁱ	−101.47 (15)
O1—Cr1—Na1—O10	−129.62 (19)	Na2—Na1—O1—Cr1ⁱ	−64.28 (14)
O1ⁱ—Cr1—Na1—O10	−56.69 (16)	O1—Cr1—O2—C1	−82.6 (3)
O3—Cr1—Na1—O10	134.18 (16)	O1ⁱ—Cr1—O2—C1	−164.0 (3)
O7—Cr1—Na1—O10	29.59 (17)	O3—Cr1—O2—C1	8.8 (3)
O6—Cr1—Na1—O10	43.99 (19)	O6—Cr1—O2—C1	100.5 (3)
Cr1ⁱ—Cr1—Na1—O10	−86.16 (14)	Cr1ⁱ—Cr1—O2—C1	−123.4 (3)
Na1ⁱ—Cr1—Na1—O10	−86.16 (14)	Na1—Cr1—O2—C1	−67.3 (3)
O2—Cr1—Na1—O8ⁱⁱⁱ	44.47 (16)	Na1ⁱ—Cr1—O2—C1	−171.6 (3)
O1—Cr1—Na1—O8ⁱⁱⁱ	66.16 (14)	O1—Cr1—O2—Na1ⁱ	89.00 (12)
O1ⁱ—Cr1—Na1—O8ⁱⁱⁱ	139.09 (11)	O1ⁱ—Cr1—O2—Na1ⁱ	7.58 (12)
O3—Cr1—Na1—O8ⁱⁱⁱ	−30.04 (12)	O3—Cr1—O2—Na1ⁱ	−179.61 (12)
O7—Cr1—Na1—O8ⁱⁱⁱ	−134.63 (15)	O6—Cr1—O2—Na1ⁱ	−87.88 (13)
O6—Cr1—Na1—O8ⁱⁱⁱ	−120.23 (14)	Cr1ⁱ—Cr1—O2—Na1ⁱ	48.20 (9)
Cr1ⁱ—Cr1—Na1—O8ⁱⁱⁱ	109.62 (9)	Na1—Cr1—O2—Na1ⁱ	104.33 (12)
Na1ⁱ—Cr1—Na1—O8ⁱⁱⁱ	109.62 (9)	O2—Cr1—O3—C2	−9.6 (3)
O2—Cr1—Na1—O9ⁱⁱⁱ	−23.14 (18)	O1—Cr1—O3—C2	84.9 (3)
O1—Cr1—Na1—O9ⁱⁱⁱ	−1.45 (14)	O1ⁱ—Cr1—O3—C2	31.6 (8)
O1ⁱ—Cr1—Na1—O9ⁱⁱⁱ	71.48 (13)	O7—Cr1—O3—C2	174.6 (3)
O3—Cr1—Na1—O9ⁱⁱⁱ	−97.65 (13)	O6—Cr1—O3—C2	−103.1 (3)
O7—Cr1—Na1—O9ⁱⁱⁱ	157.76 (17)	Cr1ⁱ—Cr1—O3—C2	77.1 (3)
O6—Cr1—Na1—O9ⁱⁱⁱ	172.16 (14)	Na1—Cr1—O3—C2	130.1 (3)
Cr1ⁱ—Cr1—Na1—O9ⁱⁱⁱ	42.01 (10)	Na1ⁱ—Cr1—O3—C2	−10.0 (3)
Na1ⁱ—Cr1—Na1—O9ⁱⁱⁱ	42.01 (10)	O2—Cr1—O6—C4	168.9 (3)
O2—Cr1—Na1—O1	−21.69 (18)	O1ⁱ—Cr1—O6—C4	79.2 (3)
O1ⁱ—Cr1—Na1—O1	72.93 (16)	O3—Cr1—O6—C4	−108.6 (3)
O3—Cr1—Na1—O1	−96.20 (15)	O7—Cr1—O6—C4	−10.9 (3)
O7—Cr1—Na1—O1	159.21 (18)	Cr1ⁱ—Cr1—O6—C4	71.2 (3)
O6—Cr1—Na1—O1	173.61 (17)	Na1—Cr1—O6—C4	−21.2 (3)
Cr1ⁱ—Cr1—Na1—O1	43.46 (12)	Na1ⁱ—Cr1—O6—C4	122.5 (3)
Na1ⁱ—Cr1—Na1—O1	43.46 (12)	O2—Cr1—O6—Na2^vi	−0.77 (18)
O2—Cr1—Na1—O7	179.10 (18)	O1ⁱ—Cr1—O6—Na2^vi	−90.48 (17)
O1—Cr1—Na1—O7	−159.21 (18)	O3—Cr1—O6—Na2^vi	81.72 (17)
O1ⁱ—Cr1—Na1—O7	−86.29 (15)	O7—Cr1—O6—Na2^vi	179.49 (18)
O3—Cr1—Na1—O7	104.59 (15)	Cr1ⁱ—Cr1—O6—Na2^vi	−98.50 (16)
O6—Cr1—Na1—O7	14.40 (17)	Na1—Cr1—O6—Na2^vi	169.10 (10)
Cr1ⁱ—Cr1—Na1—O7	−115.75 (13)	Na1ⁱ—Cr1—O6—Na2^vi	−47.15 (15)
Na1ⁱ—Cr1—Na1—O7	−115.75 (13)	O1—Cr1—O7—C3	−159.9 (3)
O2—Cr1—Na1—O2ⁱ	−93.80 (14)	O1ⁱ—Cr1—O7—C3	−78.4 (3)
O1—Cr1—Na1—O2ⁱ	−72.11 (14)	O3—Cr1—O7—C3	108.1 (3)
O1ⁱ—Cr1—Na1—O2ⁱ	0.82 (11)	O6—Cr1—O7—C3	17.0 (3)
O3—Cr1—Na1—O2ⁱ	−168.31 (11)	Cr1ⁱ—Cr1—O7—C3	−119.2 (3)
O7—Cr1—Na1—O2ⁱ	87.10 (14)	Na1—Cr1—O7—C3	−174.6 (3)
O6—Cr1—Na1—O2ⁱ	101.50 (14)	Na1ⁱ—Cr1—O7—C3	−66.9 (3)
Cr1ⁱ—Cr1—Na1—O2ⁱ	−28.65 (7)	O1—Cr1—O7—Na1	14.65 (13)
Na1ⁱ—Cr1—Na1—O2ⁱ	−28.65 (7)	O1ⁱ—Cr1—O7—Na1	96.15 (12)
O2—Cr1—Na1—C3ⁱⁱⁱ	−3.86 (17)	O3—Cr1—O7—Na1	−77.29 (13)
O1—Cr1—Na1—C3ⁱⁱⁱ	17.83 (14)	O6—Cr1—O7—Na1	−168.42 (14)
O1ⁱ—Cr1—Na1—C3ⁱⁱⁱ	90.76 (12)	Cr1ⁱ—Cr1—O7—Na1	55.41 (10)
O3—Cr1—Na1—C3ⁱⁱⁱ	−78.37 (12)	Na1ⁱ—Cr1—O7—Na1	107.64 (11)
O7—Cr1—Na1—C3ⁱⁱⁱ	177.04 (16)	O8ⁱⁱ—Na1—O7—C3	−72.9 (5)
O6—Cr1—Na1—C3ⁱⁱⁱ	−168.56 (14)	O10—Na1—O7—C3	12.3 (5)
Cr1ⁱ—Cr1—Na1—C3ⁱⁱⁱ	61.29 (9)	O8ⁱⁱⁱ—Na1—O7—C3	−137.7 (5)
Na1ⁱ—Cr1—Na1—C3ⁱⁱⁱ	61.29 (9)	O9ⁱⁱⁱ—Na1—O7—C3	132.9 (5)
O2—Cr1—Na1—C4ⁱⁱⁱ	24.11 (16)	O1—Na1—O7—C3	158.3 (5)
O1—Cr1—Na1—C4ⁱⁱⁱ	45.80 (14)	O2ⁱ—Na1—O7—C3	88.4 (5)
O1ⁱ—Cr1—Na1—C4ⁱⁱⁱ	118.73 (11)	C3ⁱⁱⁱ—Na1—O7—C3	166.4 (4)
O3—Cr1—Na1—C4ⁱⁱⁱ	−50.39 (12)	C4ⁱⁱⁱ—Na1—O7—C3	−157.6 (5)
O7—Cr1—Na1—C4ⁱⁱⁱ	−154.98 (15)	Cr1—Na1—O7—C3	170.8 (6)
O6—Cr1—Na1—C4ⁱⁱⁱ	−140.59 (14)	Cr1ⁱ—Na1—O7—C3	123.2 (5)
Cr1ⁱ—Cr1—Na1—C4ⁱⁱⁱ	89.26 (9)	Na2—Na1—O7—C3	1.0 (5)
Na1ⁱ—Cr1—Na1—C4ⁱⁱⁱ	89.27 (9)	O8ⁱⁱ—Na1—O7—Cr1	116.25 (13)
O2—Cr1—Na1—Cr1ⁱ	−65.15 (13)	O10—Na1—O7—Cr1	−158.49 (13)
O1—Cr1—Na1—Cr1ⁱ	−43.46 (12)	O8ⁱⁱⁱ—Na1—O7—Cr1	51.52 (16)
O1ⁱ—Cr1—Na1—Cr1ⁱ	29.47 (8)	O9ⁱⁱⁱ—Na1—O7—Cr1	−37.9 (3)
O3—Cr1—Na1—Cr1ⁱ	−139.66 (9)	O1—Na1—O7—Cr1	−12.47 (11)
O7—Cr1—Na1—Cr1ⁱ	115.75 (13)	O2ⁱ—Na1—O7—Cr1	−82.38 (12)
O6—Cr1—Na1—Cr1ⁱ	130.15 (12)	C3ⁱⁱⁱ—Na1—O7—Cr1	−4.4 (2)
Na1ⁱ—Cr1—Na1—Cr1ⁱ	0.0	C4ⁱⁱⁱ—Na1—O7—Cr1	31.54 (19)
O2—Cr1—Na1—Na2	−171.87 (13)	Cr1ⁱ—Na1—O7—Cr1	−47.58 (9)
O1—Cr1—Na1—Na2	−150.17 (14)	Na2—Na1—O7—Cr1	−169.83 (14)
O1ⁱ—Cr1—Na1—Na2	−77.25 (9)	O4^iv—Na2—O9—C3	144.0 (3)
O3—Cr1—Na1—Na2	113.63 (9)	O10—Na2—O9—C3	−25.2 (4)
O7—Cr1—Na1—Na2	9.04 (12)	O5^iv—Na2—O9—C3	−158.2 (3)
O6—Cr1—Na1—Na2	23.44 (13)	O6ⁱⁱ—Na2—O9—C3	67.4 (3)
Cr1ⁱ—Cr1—Na1—Na2	−106.71 (5)	C1^iv—Na2—O9—C3	171.2 (3)
Na1ⁱ—Cr1—Na1—Na2	−106.71 (5)	C2^iv—Na2—O9—C3	−167.9 (3)
O8ⁱⁱ—Na1—Na2—O9	89.19 (13)	Na1—Na2—O9—C3	−9.2 (3)
O10—Na1—Na2—O9	−159.84 (17)	Na1^vii—Na2—O9—C3	141.1 (4)
O8ⁱⁱⁱ—Na1—Na2—O9	98.03 (19)	O4^iv—Na2—O9—Na1^vii	2.8 (3)
O9ⁱⁱⁱ—Na1—Na2—O9	−140.65 (12)	O10—Na2—O9—Na1^vii	−166.37 (15)
O1—Na1—Na2—O9	−22.57 (14)	O5^iv—Na2—O9—Na1^vii	60.65 (17)
O7—Na1—Na2—O9	3.21 (12)	O6ⁱⁱ—Na2—O9—Na1^vii	−73.77 (16)
O2ⁱ—Na1—Na2—O9	−73.96 (11)	C1^iv—Na2—O9—Na1^vii	30.1 (2)
C3ⁱⁱⁱ—Na1—Na2—O9	−152.9 (3)	C2^iv—Na2—O9—Na1^vii	50.98 (19)
C4ⁱⁱⁱ—Na1—Na2—O9	124.2 (3)	C3—Na2—O9—Na1^vii	−141.1 (4)
Cr1—Na1—Na2—O9	−2.58 (10)	Na1—Na2—O9—Na1^vii	−150.31 (14)
Cr1ⁱ—Na1—Na2—O9	−53.31 (10)	Na2^v—O4—C1—O2	−170.5 (3)
O8ⁱⁱ—Na1—Na2—O4^iv	−68.17 (16)	Na2^v—O4—C1—C2	10.5 (4)
O10—Na1—Na2—O4^iv	42.79 (18)	Cr1—O2—C1—O4	174.5 (3)
O8ⁱⁱⁱ—Na1—Na2—O4^iv	−59.3 (2)	Na1ⁱ—O2—C1—O4	8.7 (7)
O9ⁱⁱⁱ—Na1—Na2—O4^iv	62.0 (2)	Cr1—O2—C1—C2	−6.5 (4)
O1—Na1—Na2—O4^iv	−179.93 (15)	Na1ⁱ—O2—C1—C2	−172.3 (3)
O7—Na1—Na2—O4^iv	−154.15 (16)	Cr1—O2—C1—Na2^v	139.7 (13)
O2ⁱ—Na1—Na2—O4^iv	128.68 (15)	Na1ⁱ—O2—C1—Na2^v	−26.1 (17)
C3ⁱⁱⁱ—Na1—Na2—O4^iv	49.8 (3)	Na2^v—O5—C2—O3	172.8 (3)
C4ⁱⁱⁱ—Na1—Na2—O4^iv	−33.1 (3)	Na2^v—O5—C2—C1	−8.3 (4)
Cr1—Na1—Na2—O4^iv	−159.94 (13)	Cr1—O3—C2—O5	−172.4 (3)
Cr1ⁱ—Na1—Na2—O4^iv	149.33 (13)	Cr1—O3—C2—C1	8.7 (4)
O8ⁱⁱ—Na1—Na2—O10	−110.96 (17)	Cr1—O3—C2—Na2^v	−141.6 (15)
O8ⁱⁱⁱ—Na1—Na2—O10	−102.1 (2)	O4—C1—C2—O5	−1.5 (6)
O9ⁱⁱⁱ—Na1—Na2—O10	19.20 (19)	O2—C1—C2—O5	179.5 (4)
O1—Na1—Na2—O10	137.27 (18)	Na2^v—C1—C2—O5	6.2 (3)
O7—Na1—Na2—O10	163.05 (17)	O4—C1—C2—O3	177.5 (4)
O2ⁱ—Na1—Na2—O10	85.88 (15)	O2—C1—C2—O3	−1.6 (5)
C3ⁱⁱⁱ—Na1—Na2—O10	7.0 (3)	Na2^v—C1—C2—O3	−174.8 (3)
C4ⁱⁱⁱ—Na1—Na2—O10	−75.9 (3)	O4—C1—C2—Na2^v	−7.7 (3)
Cr1—Na1—Na2—O10	157.27 (15)	O2—C1—C2—Na2^v	173.3 (3)
Cr1ⁱ—Na1—Na2—O10	106.54 (14)	Na2—O9—C3—O7	13.0 (6)
O8ⁱⁱ—Na1—Na2—O5^iv	166.4 (2)	Na1^vii—O9—C3—O7	156.9 (4)
O10—Na1—Na2—O5^iv	−82.7 (2)	Na2—O9—C3—C4	−167.3 (3)
O8ⁱⁱⁱ—Na1—Na2—O5^iv	175.2 (2)	Na1^vii—O9—C3—C4	−23.4 (5)
O9ⁱⁱⁱ—Na1—Na2—O5^iv	−63.5 (3)	Na2—O9—C3—Na1^vii	−144.0 (4)
O1—Na1—Na2—O5^iv	54.6 (2)	Na1^vii—O9—C3—Na2	144.0 (4)
O7—Na1—Na2—O5^iv	80.4 (2)	Cr1—O7—C3—O9	160.5 (4)
O2ⁱ—Na1—Na2—O5^iv	3.2 (2)	Na1—O7—C3—O9	−9.6 (8)
C3ⁱⁱⁱ—Na1—Na2—O5^iv	−75.7 (3)	Cr1—O7—C3—C4	−19.2 (4)
C4ⁱⁱⁱ—Na1—Na2—O5^iv	−158.6 (3)	Na1—O7—C3—C4	170.7 (3)
Cr1—Na1—Na2—O5^iv	74.6 (2)	Cr1—O7—C3—Na1^vii	−137.3 (8)
Cr1ⁱ—Na1—Na2—O5^iv	23.9 (2)	Na1—O7—C3—Na1^vii	52.6 (12)
O8ⁱⁱ—Na1—Na2—O6ⁱⁱ	10.76 (12)	Cr1—O7—C3—Na2	169.14 (17)
O10—Na1—Na2—O6ⁱⁱ	121.73 (17)	Na1—O7—C3—Na2	−1.0 (5)
O8ⁱⁱⁱ—Na1—Na2—O6ⁱⁱ	19.60 (19)	O4^iv—Na2—C3—O9	−58.6 (5)
O9ⁱⁱⁱ—Na1—Na2—O6ⁱⁱ	140.92 (17)	O10—Na2—C3—O9	158.5 (3)
O1—Na1—Na2—O6ⁱⁱ	−101.00 (13)	O5^iv—Na2—C3—O9	22.7 (3)
O7—Na1—Na2—O6ⁱⁱ	−75.22 (12)	O6ⁱⁱ—Na2—C3—O9	−107.2 (3)
O2ⁱ—Na1—Na2—O6ⁱⁱ	−152.39 (11)	C1^iv—Na2—C3—O9	−13.3 (4)
C3ⁱⁱⁱ—Na1—Na2—O6ⁱⁱ	128.7 (3)	C2^iv—Na2—C3—O9	14.5 (4)
C4ⁱⁱⁱ—Na1—Na2—O6ⁱⁱ	45.8 (3)	Na1—Na2—C3—O9	170.0 (3)
Cr1—Na1—Na2—O6ⁱⁱ	−81.01 (9)	Na1^vii—Na2—C3—O9	−25.7 (3)
Cr1ⁱ—Na1—Na2—O6ⁱⁱ	−131.74 (9)	O9—Na2—C3—O7	−169.5 (5)
O8ⁱⁱ—Na1—Na2—C1^iv	−91.3 (2)	O4^iv—Na2—C3—O7	131.9 (3)
O10—Na1—Na2—C1^iv	19.7 (2)	O10—Na2—C3—O7	−11.0 (3)
O8ⁱⁱⁱ—Na1—Na2—C1^iv	−82.5 (2)	O5^iv—Na2—C3—O7	−146.8 (2)
O9ⁱⁱⁱ—Na1—Na2—C1^iv	38.9 (3)	O6ⁱⁱ—Na2—C3—O7	83.3 (2)
O1—Na1—Na2—C1^iv	156.94 (19)	C1^iv—Na2—C3—O7	177.1 (3)
O7—Na1—Na2—C1^iv	−177.3 (2)	C2^iv—Na2—C3—O7	−155.1 (2)
O2ⁱ—Na1—Na2—C1^iv	105.5 (2)	Na1—Na2—C3—O7	0.4 (2)
C3ⁱⁱⁱ—Na1—Na2—C1^iv	26.6 (3)	Na1^vii—Na2—C3—O7	164.8 (3)
C4ⁱⁱⁱ—Na1—Na2—C1^iv	−56.3 (3)	O9—Na2—C3—C4	32.6 (7)
Cr1—Na1—Na2—C1^iv	176.93 (18)	O4^iv—Na2—C3—C4	−26.0 (10)
Cr1ⁱ—Na1—Na2—C1^iv	126.20 (18)	O10—Na2—C3—C4	−168.9 (8)
O8ⁱⁱ—Na1—Na2—C2^iv	−149.3 (3)	O5^iv—Na2—C3—C4	55.3 (8)
O10—Na1—Na2—C2^iv	−38.4 (3)	O6ⁱⁱ—Na2—C3—C4	−74.6 (8)
O8ⁱⁱⁱ—Na1—Na2—C2^iv	−140.5 (3)	C1^iv—Na2—C3—C4	19.2 (9)
O9ⁱⁱⁱ—Na1—Na2—C2^iv	−19.2 (3)	C2^iv—Na2—C3—C4	47.0 (8)
O1—Na1—Na2—C2^iv	98.9 (3)	Na1—Na2—C3—C4	−157.5 (8)
O7—Na1—Na2—C2^iv	124.7 (3)	Na1^vii—Na2—C3—C4	6.9 (7)
O2ⁱ—Na1—Na2—C2^iv	47.5 (3)	O9—Na2—C3—Na1^vii	25.7 (3)
C3ⁱⁱⁱ—Na1—Na2—C2^iv	−31.4 (4)	O4^iv—Na2—C3—Na1^vii	−32.9 (3)
C4ⁱⁱⁱ—Na1—Na2—C2^iv	−114.3 (4)	O10—Na2—C3—Na1^vii	−175.79 (12)
Cr1—Na1—Na2—C2^iv	118.9 (3)	O5^iv—Na2—C3—Na1^vii	48.39 (13)
Cr1ⁱ—Na1—Na2—C2^iv	68.2 (3)	O6ⁱⁱ—Na2—C3—Na1^vii	−81.51 (11)
O8ⁱⁱ—Na1—Na2—C3	85.74 (12)	C1^iv—Na2—C3—Na1^vii	12.4 (3)
O10—Na1—Na2—C3	−163.30 (17)	C2^iv—Na2—C3—Na1^vii	40.15 (17)
O8ⁱⁱⁱ—Na1—Na2—C3	94.57 (19)	Na1—Na2—C3—Na1^vii	−164.35 (11)
O9ⁱⁱⁱ—Na1—Na2—C3	−144.10 (18)	Na1^vi—O8—C4—O6	32.1 (7)
O1—Na1—Na2—C3	−26.02 (13)	Na1^vii—O8—C4—O6	−170.9 (4)
O7—Na1—Na2—C3	−0.24 (12)	Na1^vi—O8—C4—C3	−148.0 (3)
O2ⁱ—Na1—Na2—C3	−77.41 (11)	Na1^vii—O8—C4—C3	9.0 (5)
C3ⁱⁱⁱ—Na1—Na2—C3	−156.3 (2)	Na1^vi—O8—C4—Na1^vii	−157.0 (5)
C4ⁱⁱⁱ—Na1—Na2—C3	120.8 (3)	Cr1—O6—C4—O8	−176.3 (4)
Cr1—Na1—Na2—C3	−6.03 (9)	Na2^vi—O6—C4—O8	−7.4 (6)
Cr1ⁱ—Na1—Na2—C3	−56.76 (10)	Cr1—O6—C4—C3	3.7 (4)
O8ⁱⁱ—Na1—Na2—Na1^vii	73.21 (9)	Na2^vi—O6—C4—C3	172.7 (3)
O10—Na1—Na2—Na1^vii	−175.83 (16)	Cr1—O6—C4—Na1^vii	147.1 (15)
O8ⁱⁱⁱ—Na1—Na2—Na1^vii	82.04 (16)	Na2^vi—O6—C4—Na1^vii	−43.9 (18)
O9ⁱⁱⁱ—Na1—Na2—Na1^vii	−156.63 (15)	O9—C3—C4—O8	10.8 (6)
O1—Na1—Na2—Na1^vii	−38.55 (12)	O7—C3—C4—O8	−169.4 (4)
O7—Na1—Na2—Na1^vii	−12.77 (9)	Na1^vii—C3—C4—O8	−6.6 (4)
O2ⁱ—Na1—Na2—Na1^vii	−89.94 (9)	Na2—C3—C4—O8	−13.6 (10)
C3ⁱⁱⁱ—Na1—Na2—Na1^vii	−168.9 (3)	O9—C3—C4—O6	−169.3 (4)
C4ⁱⁱⁱ—Na1—Na2—Na1^vii	108.2 (3)	O7—C3—C4—O6	10.5 (5)
Cr1—Na1—Na2—Na1^vii	−18.56 (6)	Na1^vii—C3—C4—O6	173.3 (4)
Cr1ⁱ—Na1—Na2—Na1^vii	−69.29 (7)	Na2—C3—C4—O6	166.3 (6)
O2—Cr1—O1—Cr1ⁱ	−88.64 (13)	O9—C3—C4—Na1^vii	17.4 (4)
O1ⁱ—Cr1—O1—Cr1ⁱ	0.0	O7—C3—C4—Na1^vii	−162.9 (4)
O3—Cr1—O1—Cr1ⁱ	−171.14 (13)	Na2—C3—C4—Na1^vii	−7.0 (8)
O7—Cr1—O1—Cr1ⁱ	90.88 (13)	O9—Na2—O10—Na1	24.5 (2)
Na1—Cr1—O1—Cr1ⁱ	105.65 (14)	O4^iv—Na2—O10—Na1	−148.41 (13)
Na1ⁱ—Cr1—O1—Cr1ⁱ	−42.17 (10)	O5^iv—Na2—O10—Na1	139.64 (15)
O2—Cr1—O1—Na1	165.71 (12)	O6ⁱⁱ—Na2—O10—Na1	−56.63 (15)
O1ⁱ—Cr1—O1—Na1	−105.65 (14)	C1^iv—Na2—O10—Na1	−168.56 (13)
O3—Cr1—O1—Na1	83.21 (13)	C2^iv—Na2—O10—Na1	163.34 (14)
O7—Cr1—O1—Na1	−14.77 (13)	C3—Na2—O10—Na1	15.75 (16)
Cr1ⁱ—Cr1—O1—Na1	−105.65 (14)	Na1^vii—Na2—O10—Na1	8.7 (3)
Na1ⁱ—Cr1—O1—Na1	−147.82 (8)	O8ⁱⁱ—Na1—O10—Na2	61.46 (14)
O8ⁱⁱ—Na1—O1—Cr1	−47.71 (16)	O8ⁱⁱⁱ—Na1—O10—Na2	126.21 (16)
O10—Na1—O1—Cr1	90.3 (2)	O9ⁱⁱⁱ—Na1—O10—Na2	−166.65 (13)
O8ⁱⁱⁱ—Na1—O1—Cr1	−110.77 (13)	O1—Na1—O10—Na2	−82.6 (2)
O9ⁱⁱⁱ—Na1—O1—Cr1	178.69 (13)	O7—Na1—O10—Na2	−15.28 (15)
O7—Na1—O1—Cr1	12.59 (11)	O2ⁱ—Na1—O10—Na2	−86.80 (13)
O2ⁱ—Na1—O1—Cr1	94.84 (13)	C3ⁱⁱⁱ—Na1—O10—Na2	−176.89 (13)
C3ⁱⁱⁱ—Na1—O1—Cr1	−161.83 (14)	C4ⁱⁱⁱ—Na1—O10—Na2	154.08 (14)
C4ⁱⁱⁱ—Na1—O1—Cr1	−131.45 (14)	Cr1—Na1—O10—Na2	−31.93 (19)
Cr1ⁱ—Na1—O1—Cr1	101.47 (15)	Cr1ⁱ—Na1—O10—Na2	−89.20 (12)
Na2—Na1—O1—Cr1	37.20 (16)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O11—H11B···O9ⁱⁱ	0.88 (2)	2.23 (2)	3.080 (5)	163 (5)
O11—H11A···O6	0.88 (4)	2.53 (4)	3.144 (5)	128 (4)
O11—H11A···O3	0.88 (4)	2.25 (4)	2.949 (4)	137 (4)
O10—H10B···O5^viii	0.88 (4)	2.36 (4)	3.123 (4)	144 (5)
O10—H10A···O5^ix	0.91 (2)	2.02 (2)	2.922 (5)	179 (4)
O1—H1···O11ⁱⁱⁱ	0.85	2.01	2.808 (4)	156

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

Experimental details

Crystal data
Chemical formula	[CrNa₂(C₂O₄)₂(OH)(H₂O)]·H₂O
M_r	327.06
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	173
a, b, c (Å)	9.4776 (10), 8.603 (1), 12.5353 (14)
β (°)	102.503 (2)
V (Å³)	997.84 (19)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.29
Crystal size (mm)	0.60 × 0.12 × 0.10

Data collection
Diffractometer	Bruker–Nonius X8 Kappa APEXII CCD area-detector
Absorption correction	Multi-scan (APEX2; Bruker 2005)
T_min, T_max	0.832, 0.882
No. of measured, independent and observed [I > 2σ(I)] reflections	13658, 2018, 1625
R_int	0.037
(sin θ/λ)_max (Å⁻¹)	0.625

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.044, 0.133, 1.14
No. of reflections	2018
No. of parameters	175
No. of restraints	6
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.85, −0.80

Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SIR2002 (Burla et al., 2003), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O11—H11B···O9ⁱ	0.879 (19)	2.23 (2)	3.080 (5)	163 (5)
O11—H11A···O6	0.88 (4)	2.53 (4)	3.144 (5)	128 (4)
O11—H11A···O3	0.88 (4)	2.25 (4)	2.949 (4)	137 (4)
O10—H10B···O5ⁱⁱ	0.88 (4)	2.36 (4)	3.123 (4)	144 (5)
O10—H10A···O5ⁱⁱⁱ	0.905 (19)	2.02 (2)	2.922 (5)	179 (4)
O1—H1···O11^iv	0.85	2.01	2.808 (4)	156.3

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

Acknowledgements

The authors thank Dr Y. A. Mbiangué for his help with the chemical structural drawing. Financial support from the Junta de Andalucía (Project P09-FQM-4826) and CSIC (PIF08–017-1) is gratefully acknowledged.

References

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