Octa­aqua­bis­[di­hydrogen 1,2,4,5-benzene­tetra­carboxyl­ate(2-)]­disodium(I)­zinc(II) dihydrate

The title compound, [Na₂Zn(C₁₀H₄O₈)₂(H₂O)₈]·2H₂O, consists of six-coordinated Zn²⁺ and Na⁺ cations, aqua ligands, crystal water mol­ecules and di­hydrogen 1,2,4,5-benzene­tetra­carboxyl­ate(2-) (H₂btc) anions. The six-coordinated zinc centers, which are situated at the inversion center, are linked into one-dimensional chains via six coordinated sodium ions in pairs and extended further into a three-dimensional framework via hydrogen bonding.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.056
• wR factor = 0.163
• Data-to-parameter ratio = 9.7

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



PLAT_369  Alert C Long   C(sp2)-C(sp2) Bond  C(2)   -   C(4)   =       1.53 Ang.

PLAT_369  Alert C Long   C(sp2)-C(sp2) Bond  C(5)   -   C(6)   =       1.53 Ang.

PLAT_742  Alert C Angle   Calc    90.00(3), Rep       90.00 ....    Missing s.u.
                     O1   -ZN1  -O3      1.555   1.555   1.555

PLAT_742  Alert C Angle   Calc    90.00(3), Rep       90.00 ....    Missing s.u.
                     O1   -ZN1  -O2      1.555   1.555   1.555

PLAT_742  Alert C Angle   Calc    90.00(3), Rep       90.00 ....    Missing s.u.
                     O1   -ZN1  -NA1     1.555   1.555   1.555


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 5 Alert Level C = Please check

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Computing details

Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: CAD-4 Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXL97; software used to prepare material for publication: SHELXL97.

Octaaquabis[dihydrogen 1,2,4,5-benzenetetracarboxylate(2-)]dissodium(I)zinc(II) dihydrate

Crystal data

[Na2Zn(C10H4O8)2(H2O)8]·2H2O	F(000) = 816
Mr = 795.77	Dx = 1.768 Mg m^−3
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71073 Å
a = 7.2861 (15) Å	Cell parameters from 25 reflections
b = 20.179 (4) Å	θ = 13.1–14.8°
c = 10.453 (2) Å	µ = 0.96 mm^−1
β = 103.47 (3)°	T = 293 K
V = 1494.5 (5) Å^3	Prism, colorless
Z = 2	0.46 × 0.13 × 0.05 mm

Data collection

Enraf-Nonius CAD-4-II diffractometer	1253 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.024
Graphite monochromator	θmax = 26.0°, θmin = 2.0°
ω–2θ scans	h = 0→8
Absorption correction: ψ scan (North et al., 1968)	k = −24→0
Tmin = 0.684, Tmax = 0.998	l = −12→12
1633 measured reflections	3 standard reflections every 300 reflections
1511 independent reflections	intensity decay: 2.5%

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)] = 0.056	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.163	w = 1/[σ^2(Fo^2) + (0.0965P)^2 + 0.721P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max < 0.001
1511 reflections	Δρmax = 0.93 e Å^−3
156 parameters	Δρmin = −1.74 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0061 (14)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.0000	0.5000	0.0000	0.0248 (4)
Na1	−0.3159 (4)	0.5000	−0.3275 (2)	0.0366 (6)
O1	0.0000	0.3987 (2)	0.0000	0.0357 (11)
H1A	0.0627	0.3711	0.0505	0.053*
O2	0.0284 (7)	0.5000	−0.1976 (4)	0.0335 (11)
H2A	0.074 (8)	0.471 (2)	−0.217 (5)	0.050*
O3	−0.2922 (6)	0.5000	−0.0845 (4)	0.0300 (9)
H3A	−0.342 (8)	0.530 (2)	−0.060 (5)	0.045*
O4	−0.3311 (9)	0.5000	−0.5641 (5)	0.0505 (14)
H4A	−0.3022	0.5319	−0.6014	0.076*
O5	−0.2010 (5)	0.81208 (17)	−0.1730 (3)	0.0503 (10)
H56	−0.194 (9)	0.751 (4)	−0.178 (6)	0.075*
O6	−0.1996 (5)	0.69391 (16)	−0.1729 (3)	0.0494 (10)
O7	−0.3064 (5)	0.61205 (15)	−0.3032 (3)	0.0473 (9)
O8	−0.3100 (4)	0.89564 (14)	−0.3015 (3)	0.0360 (8)
O101	−0.5000	0.5955 (2)	0.0000	0.0325 (10)
H10A	−0.4410	0.6229	0.0552	0.049*
C1	−0.5000	0.8207 (3)	−0.5000	0.0229 (11)
H1	−0.5000	0.865 (3)	−0.5000	0.026 (15)*
C2	−0.3969 (5)	0.71872 (17)	−0.3887 (4)	0.0214 (8)
C3	−0.5000	0.6868 (3)	−0.5000	0.0251 (12)
H3	−0.5000	0.641 (3)	−0.5000	0.015 (13)*
C4	−0.2960 (6)	0.67071 (19)	−0.2820 (4)	0.0291 (9)
C5	−0.2965 (6)	0.83554 (19)	−0.2802 (4)	0.0264 (9)
C6	−0.3967 (5)	0.78863 (18)	−0.3886 (3)	0.0209 (8)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0311 (6)	0.0200 (5)	0.0217 (5)	0.000	0.0026 (4)	0.000
Na1	0.0550 (17)	0.0197 (12)	0.0301 (13)	0.000	−0.0006 (12)	0.000
O1	0.045 (3)	0.018 (2)	0.031 (2)	0.000	−0.0167 (19)	0.000
O2	0.050 (3)	0.020 (2)	0.032 (2)	0.000	0.013 (2)	0.000
O3	0.034 (2)	0.023 (2)	0.032 (2)	0.000	0.0051 (18)	0.000
O4	0.079 (4)	0.031 (3)	0.049 (3)	0.000	0.030 (3)	0.000
O5	0.071 (3)	0.0287 (18)	0.0336 (17)	−0.0028 (16)	−0.0228 (17)	−0.0042 (13)
O6	0.069 (3)	0.0265 (18)	0.0351 (18)	0.0011 (15)	−0.0234 (17)	0.0029 (13)
O7	0.068 (2)	0.0194 (17)	0.0423 (18)	0.0041 (14)	−0.0118 (17)	0.0032 (13)
O8	0.053 (2)	0.0209 (15)	0.0304 (15)	−0.0024 (13)	0.0024 (14)	−0.0047 (12)
O101	0.038 (2)	0.021 (2)	0.031 (2)	0.000	−0.0086 (18)	0.000
C1	0.029 (3)	0.013 (2)	0.025 (3)	0.000	0.003 (2)	0.000
C2	0.0236 (19)	0.0185 (18)	0.0204 (18)	0.0008 (15)	0.0019 (15)	0.0028 (14)
C3	0.030 (3)	0.017 (3)	0.026 (3)	0.000	0.001 (2)	0.000
C4	0.031 (2)	0.023 (2)	0.029 (2)	0.0032 (17)	−0.0011 (16)	0.0032 (17)
C5	0.028 (2)	0.023 (2)	0.0253 (19)	−0.0024 (16)	0.0012 (16)	−0.0039 (16)
C6	0.0212 (19)	0.0205 (18)	0.0199 (18)	0.0004 (14)	0.0023 (15)	−0.0013 (14)

Geometric parameters (Å, º)

Zn1—O1	2.045 (4)	O3—H3A	0.78 (5)
Zn1—O1^i	2.045 (4)	O4—H4A	0.81 (6)
Zn1—O3^i	2.106 (4)	O5—C5	1.264 (5)
Zn1—O3	2.106 (4)	O5—H56	1.24 (7)
Zn1—O2^i	2.123 (4)	O6—C4	1.281 (5)
Zn1—O2	2.123 (4)	O6—H56	1.15 (7)
Zn1—Na1^i	3.653 (3)	O7—C4	1.203 (5)
Zn1—Na1	3.653 (3)	O8—C5	1.233 (5)
Na1—O7^ii	2.274 (3)	O101—H10A	0.84 (5)
Na1—O7	2.274 (3)	C1—C6^iv	1.390 (4)
Na1—O4	2.449 (6)	C1—C6	1.390 (4)
Na1—O3	2.505 (5)	C1—H1	0.90 (6)
Na1—O4^iii	2.558 (7)	C2—C3	1.388 (4)
Na1—O2	2.559 (6)	C2—C6	1.411 (5)
Na1—Na1^iii	3.962 (5)	C2—C4	1.530 (5)
O4—Na1^iii	2.558 (7)	C3—C2^iv	1.388 (4)
O1—H1A	0.83 (5)	C3—H3	0.92 (5)
O2—H2A	0.73 (5)	C5—C6	1.526 (5)
O1—Zn1—O1^i	180.00	O7—Na1—Zn1	84.2 (1)
O1—Zn1—O3^i	90.00	O4—Na1—Zn1	144.7 (2)
O1^i—Zn1—O3^i	90.00	O3—Na1—Zn1	33.9 (1)
O1—Zn1—O3	90.00	O4^iii—Na1—Zn1	139.9 (1)
O1^i—Zn1—O3	90.00	O2—Na1—Zn1	34.6 (1)
O3^i—Zn1—O3	180.0	O7^ii—Na1—Na1^iii	95.6 (1)
O1—Zn1—O2^i	90.0	O7—Na1—Na1^iii	95.6 (1)
O1^i—Zn1—O2^i	90.0	O4—Na1—Na1^iii	38.7 (2)
O3^i—Zn1—O2^i	84.8 (2)	O3—Na1—Na1^iii	142.7 (2)
O3—Zn1—O2^i	95.2 (2)	O4^iii—Na1—Na1^iii	36.7 (1)
O1—Zn1—O2	90.0	O2—Na1—Na1^iii	148.8 (2)
O1^i—Zn1—O2	90.0	Zn1—Na1—Na1^iii	176.6 (1)
O3^i—Zn1—O2	95.2 (2)	Zn1—O1—H1A	132 (4)
O3—Zn1—O2	84.8 (2)	O6^i—O1—H1A	2 (4)
O2^i—Zn1—O2	180.00	Zn1—O2—Na1	102.2 (2)
O1—Zn1—Na1^i	90.0	Na1—O2—H2A	108 (5)
O1^i—Zn1—Na1^i	90.0	Zn1—O3—Na1	104.4 (2)
O3^i—Zn1—Na1^i	41.6 (1)	Zn1—O3—H3A	111 (4)
O3—Zn1—Na1^i	138.4 (1)	Na1—O3—H3A	114 (4)
O2^i—Zn1—Na1^i	43.2 (1)	Na1—O4—Na1^iii	104.6 (2)
O2—Zn1—Na1^i	136.8 (1)	C4—O7—Na1	175.8 (3)
O1—Zn1—Na1	90.0	Na1—O4—H4A	122 (5)
O1^i—Zn1—Na1	90.0	Na1^iii—O4—H4A	98 (5)
O3^i—Zn1—Na1	138.4 (1)	C5—O5—H56	111 (3)
O3—Zn1—Na1	41.6 (1)	C4—O6—H56	110 (3)
O2^i—Zn1—Na1	136.8 (1)	C6^iv—C1—C6	124.5 (5)
O2—Zn1—Na1	43.2 (1)	C6^iv—C1—H1	117.7 (3)
Na1^i—Zn1—Na1	180.0	C6—C1—H1	117.7 (2)
O7^ii—Na1—O7	167.6 (2)	C3—C2—C6	117.7 (4)
O7^ii—Na1—O4	96.1 (1)	C3—C2—C4	113.0 (4)
O7—Na1—O4	96.1 (1)	C6—C2—C4	129.3 (3)
O7^ii—Na1—O3	83.9 (1)	C2—C3—C2^iv	124.6 (5)
O7—Na1—O3	83.9 (1)	C2—C3—H3	117.7 (3)
O4—Na1—O3	178.7 (2)	C2^iv—C3—H3	117.7 (3)
O7^ii—Na1—O4^iii	92.9 (1)	O7—C4—O6	121.4 (4)
O7—Na1—O4^iii	92.9 (1)	O7—C4—C2	119.3 (4)
O4—Na1—O4^iii	75.4 (2)	O6—C4—C2	119.2 (3)
O3—Na1—O4^iii	105.9 (2)	O8—C5—O5	122.2 (4)
O7^ii—Na1—O2	86.6 (1)	O8—C5—C6	118.2 (3)
O7—Na1—O2	86.6 (1)	O5—C5—C6	119.7 (4)
O4—Na1—O2	110.1 (2)	C1—C6—C2	117.7 (4)
O3—Na1—O2	68.6 (2)	C1—C6—C5	113.9 (3)
O4^iii—Na1—O2	174.5 (2)	C2—C6—C5	128.4 (3)
O7^ii—Na1—Zn1	84.2 (1)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···O6^i	0.83	1.94	2.765 (4)	177
O3—H3A···O101	0.78 (5)	1.95 (5)	2.722 (4)	170 (5)
O2—H2A···O8^v	0.73 (5)	2.03 (5)	2.756 (4)	171 (6)
O4—H4A···O8^vi	0.81	2.06	2.853 (5)	171
O6—H56···O5	1.15 (7)	1.24 (7)	2.384 (5)	172 (6)
O101—H10A···O5^vii	0.84	1.93	2.768 (4)	176

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