Poly[di-μ9-citrato-tetra-sodiumzinc].

In the title compound, [Na4Zn(C6H5O7)2] n , the Zn(II) ion lies on an inversion center and is coordinated by six O atoms from two citrate ligands, forming a distorted octa-hedral geometry. There are two crystallographically independent Na(+) cations in the asymmetric unit. One Na(+) cation exhibits a distorted square-pyramidal geometry defined by five O atoms from four citrate ligands. The other Na(+) cation is surrounded by six O atoms from five citrate ligands in a distorted octa-hedral geometry. The Na(+) cations are bridged by citrate carboxyl-ate groups, forming a layer parallel to (100). The layers are further assembled into a three-dimensional network with the [Zn(citrate)2](4-) building units as 'pillars'; O-H⋯O hydrogen bonds also stabilize the structure.

Related literature

For an isotypic compound, see: Liu et al. (2012 ▶).

Experimental

Crystal data

[Na4Zn(C6H5O7)2]

M = 535.55

Monoclinic,

a = 7.9642 (16) Å

b = 12.530 (3) Å

c = 8.7090 (17) Å

β = 113.66 (3)°

V = 796.0 (3) Å3

Z = 2

Mo Kα radiation

μ = 1.74 mm−1

T = 293 K

0.21 × 0.21 × 0.20 mm

Data collection

Rigaku SCXmini CCD diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.712, T max = 0.722

8270 measured reflections

1831 independent reflections

1570 reflections with I > 2σ(I)

R int = 0.048

Refinement

R[F 2 > 2σ(F 2)] = 0.037

wR(F 2) = 0.075

S = 1.15

1831 reflections

145 parameters

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.37 e Å−3

Δρmin = −0.47 e Å−3

Data collection: CrystalClear (Rigaku, 2005 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶) and DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablock(s) I. DOI: 10.1107/S1600536813030067/hy2639sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813030067/hy2639Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Na4Zn(C6H5O7)2]	F(000) = 536
Mr = 535.55	Dx = 2.234 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 7740 reflections
a = 7.9642 (16) Å	θ = 3.0–27.5°
b = 12.530 (3) Å	µ = 1.74 mm−1
c = 8.7090 (17) Å	T = 293 K
β = 113.66 (3)°	Block, colorless
V = 796.0 (3) Å3	0.21 × 0.21 × 0.20 mm
Z = 2

Rigaku SCXmini CCD diffractometer	1831 independent reflections
Radiation source: fine-focus sealed tube	1570 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.048
ω scan	θmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −10→10
Tmin = 0.712, Tmax = 0.722	k = −16→16
8270 measured reflections	l = −11→11

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)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.075	H atoms treated by a mixture of independent and constrained refinement
S = 1.15	w = 1/[σ2(Fo2) + (0.0289P)2 + 0.3351P] where P = (Fo2 + 2Fc2)/3
1831 reflections	(Δ/σ)max = 0.001
145 parameters	Δρmax = 0.37 e Å−3
0 restraints	Δρmin = −0.47 e Å−3

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.

	x	y	z	Uiso*/Ueq
O7	0.4930 (2)	0.98761 (13)	0.7363 (2)	0.0127 (4)
O3	0.2766 (2)	0.89905 (13)	0.4482 (2)	0.0178 (4)
O4	0.1751 (2)	0.77628 (13)	0.5749 (2)	0.0175 (4)
O6	0.8225 (3)	0.72885 (15)	0.7149 (2)	0.0233 (4)
O5	0.6783 (2)	0.87114 (13)	0.5716 (2)	0.0175 (4)
C8	0.7041 (3)	0.8007 (2)	0.6829 (3)	0.0141 (5)
C4	0.2806 (3)	0.84956 (19)	0.5774 (3)	0.0124 (5)
C5	0.5911 (3)	0.80021 (19)	0.7885 (3)	0.0132 (5)
H5A	0.6748	0.8118	0.9042	0.016*
H5B	0.5407	0.7291	0.7822	0.016*
C3	0.4328 (3)	0.87982 (18)	0.7479 (3)	0.0118 (5)
C2	0.3615 (3)	0.87711 (19)	0.8861 (3)	0.0144 (5)
H2A	0.3180	0.8056	0.8920	0.017*
H2B	0.4629	0.8916	0.9923	0.017*
O2	0.1969 (2)	0.98895 (14)	0.9984 (2)	0.0179 (4)
Zn1	0.5000	1.0000	0.5000	0.01321 (12)
Na2	−0.05408 (14)	1.12137 (8)	0.83937 (13)	0.0216 (3)
Na1	0.10230 (14)	1.11830 (8)	0.53517 (13)	0.0222 (3)
O1	0.1002 (2)	0.98321 (13)	0.7212 (2)	0.0186 (4)
C1	0.2085 (3)	0.95534 (19)	0.8644 (3)	0.0131 (5)
H1	0.606 (4)	1.000 (2)	0.828 (4)	0.016*

	U11	U22	U33	U12	U13	U23
O7	0.0154 (9)	0.0111 (9)	0.0118 (9)	−0.0021 (7)	0.0057 (7)	−0.0007 (7)
O3	0.0185 (9)	0.0207 (10)	0.0114 (9)	−0.0038 (8)	0.0030 (8)	0.0027 (7)
O4	0.0173 (9)	0.0160 (9)	0.0210 (10)	−0.0047 (7)	0.0095 (8)	−0.0030 (7)
O6	0.0225 (10)	0.0256 (11)	0.0245 (11)	0.0128 (8)	0.0123 (9)	0.0071 (8)
O5	0.0223 (10)	0.0168 (9)	0.0180 (9)	0.0037 (7)	0.0127 (8)	0.0041 (7)
C8	0.0123 (12)	0.0156 (13)	0.0137 (12)	0.0008 (10)	0.0045 (10)	−0.0014 (10)
C4	0.0110 (12)	0.0132 (12)	0.0151 (12)	0.0031 (9)	0.0072 (10)	−0.0014 (9)
C5	0.0145 (12)	0.0127 (12)	0.0131 (12)	0.0023 (10)	0.0065 (10)	0.0017 (9)
C3	0.0136 (12)	0.0104 (11)	0.0123 (12)	−0.0003 (9)	0.0062 (10)	0.0028 (9)
C2	0.0155 (12)	0.0160 (13)	0.0134 (13)	0.0014 (10)	0.0076 (11)	0.0024 (10)
O2	0.0176 (9)	0.0229 (10)	0.0162 (9)	0.0018 (8)	0.0098 (8)	−0.0047 (7)
Zn1	0.0152 (2)	0.0130 (2)	0.0124 (2)	0.00022 (17)	0.00663 (17)	0.00209 (16)
Na2	0.0197 (5)	0.0236 (6)	0.0216 (6)	0.0023 (4)	0.0084 (5)	−0.0013 (4)
Na1	0.0208 (6)	0.0253 (6)	0.0223 (6)	−0.0022 (4)	0.0105 (5)	−0.0007 (4)
O1	0.0178 (9)	0.0208 (10)	0.0159 (9)	0.0024 (7)	0.0053 (8)	0.0006 (7)
C1	0.0134 (12)	0.0113 (11)	0.0165 (13)	−0.0039 (10)	0.0080 (11)	−0.0011 (10)

O7—C3	1.450 (3)	O2—Na2	2.539 (2)
O7—Zn1	2.0866 (17)	Zn1—O5iv	2.0742 (17)
O3—C4	1.274 (3)	Zn1—O3iv	2.0796 (17)
O3—Zn1	2.0796 (17)	Zn1—O7iv	2.0866 (17)
O3—Na2i	2.432 (2)	Na2—O4v	2.415 (2)
O4—C4	1.239 (3)	Na2—O3i	2.432 (2)
O4—Na2ii	2.415 (2)	Na2—O6vi	2.478 (2)
O4—Na1i	2.417 (2)	Na2—O2vii	2.548 (2)
O6—C8	1.251 (3)	Na2—O1	2.565 (2)
O6—Na1iii	2.443 (2)	Na1—O5iv	2.288 (2)
O6—Na2iii	2.478 (2)	Na1—O1	2.348 (2)
O5—C8	1.266 (3)	Na1—O4i	2.417 (2)
O5—Zn1	2.0742 (17)	Na1—O6vi	2.443 (2)
O5—Na1iv	2.288 (2)	Na1—O1i	2.512 (2)
C8—C5	1.523 (3)	Na1—C4i	2.833 (3)
C8—Na1iv	3.061 (3)	Na1—C8iv	3.061 (3)
C4—C3	1.540 (3)	O1—C1	1.248 (3)
C4—Na1i	2.833 (3)	O7—H1	0.95 (3)
C5—C3	1.534 (3)	C2—H2A	0.97
C3—C2	1.523 (3)	C2—H2B	0.97
C2—C1	1.516 (3)	C5—H5A	0.97
O2—C1	1.279 (3)	C5—H5B	0.97
C3—O7—Zn1	106.16 (13)	Na1—Na2—Na1viii	102.34 (4)
C4—O3—Zn1	112.86 (16)	O4v—Na2—Na2vii	113.39 (6)
C4—O3—Na2i	127.44 (16)	O3i—Na2—Na2vii	120.36 (6)
Zn1—O3—Na2i	119.59 (8)	O6vi—Na2—Na2vii	125.52 (7)
C4—O4—Na2ii	160.44 (17)	O2—Na2—Na2vii	38.48 (4)
C4—O4—Na1i	96.18 (14)	O2vii—Na2—Na2vii	38.32 (4)
Na2ii—O4—Na1i	98.47 (7)	O1—Na2—Na2vii	76.31 (5)
C8—O6—Na1iii	119.97 (16)	Na1—Na2—Na2vii	120.15 (4)
C8—O6—Na2iii	154.24 (17)	Na1viii—Na2—Na2vii	114.57 (5)
Na1iii—O6—Na2iii	85.80 (7)	O5iv—Na1—O1	122.68 (8)
C8—O5—Zn1	130.84 (16)	O5iv—Na1—O4i	122.16 (7)
C8—O5—Na1iv	115.86 (16)	O1—Na1—O4i	114.15 (7)
Zn1—O5—Na1iv	112.04 (8)	O5iv—Na1—O6vi	112.02 (8)
O6—C8—O5	123.2 (2)	O1—Na1—O6vi	82.02 (7)
O6—C8—C5	116.0 (2)	O4i—Na1—O6vi	84.37 (8)
O5—C8—C5	120.8 (2)	O5iv—Na1—O1i	89.47 (7)
O4—C4—O3	124.7 (2)	O1—Na1—O1i	93.91 (7)
O4—C4—C3	117.7 (2)	O4i—Na1—O1i	76.45 (7)
O3—C4—C3	117.6 (2)	O6vi—Na1—O1i	156.79 (8)
C8—C5—C3	119.2 (2)	O5iv—Na1—C4i	137.95 (8)
O7—C3—C2	108.32 (19)	O1—Na1—C4i	92.09 (8)
O7—C3—C5	110.93 (19)	O4i—Na1—C4i	25.78 (6)
C2—C3—C5	109.63 (19)	O6vi—Na1—C4i	94.17 (8)
O7—C3—C4	108.45 (18)	O1i—Na1—C4i	63.03 (7)
C2—C3—C4	110.9 (2)	O5iv—Na1—C8iv	21.85 (6)
C5—C3—C4	108.56 (19)	O1—Na1—C8iv	144.32 (8)
C1—C2—C3	115.0 (2)	O4i—Na1—C8iv	100.39 (7)
C1—O2—Na2	92.67 (15)	O6vi—Na1—C8iv	111.12 (7)
C1—O2—Na2vii	122.64 (15)	O1i—Na1—C8iv	85.42 (7)
Na2—O2—Na2vii	103.20 (7)	C4i—Na1—C8iv	118.60 (8)
O5iv—Zn1—O5	180.0	O5iv—Na1—Na1i	112.02 (7)
O5iv—Zn1—O3iv	90.85 (7)	O1—Na1—Na1i	49.04 (5)
O5—Zn1—O3iv	89.15 (7)	O4i—Na1—Na1i	96.43 (6)
O5iv—Zn1—O3	89.15 (7)	O6vi—Na1—Na1i	126.69 (7)
O5—Zn1—O3	90.85 (7)	O1i—Na1—Na1i	44.88 (5)
O3iv—Zn1—O3	180.000 (1)	C4i—Na1—Na1i	71.49 (6)
O5iv—Zn1—O7iv	86.09 (7)	C8iv—Na1—Na1i	120.93 (7)
O5—Zn1—O7iv	93.91 (7)	O5iv—Na1—Na2	155.15 (7)
O3iv—Zn1—O7iv	79.02 (7)	O1—Na1—Na2	49.81 (5)
O3—Zn1—O7iv	100.98 (7)	O4i—Na1—Na2	74.74 (5)
O5iv—Zn1—O7	93.91 (7)	O6vi—Na1—Na2	47.54 (5)
O5—Zn1—O7	86.09 (7)	O1i—Na1—Na2	113.50 (6)
O3iv—Zn1—O7	100.98 (7)	C4i—Na1—Na2	65.27 (6)
O3—Zn1—O7	79.02 (7)	C8iv—Na1—Na2	157.96 (6)
O7iv—Zn1—O7	180.000 (1)	Na1i—Na1—Na2	81.11 (4)
O5iv—Zn1—Na1	35.88 (5)	O5iv—Na1—Zn1	32.08 (5)
O5—Zn1—Na1	144.12 (5)	O1—Na1—Zn1	90.68 (6)
O3iv—Zn1—Na1	115.73 (5)	O4i—Na1—Zn1	151.83 (6)
O3—Zn1—Na1	64.27 (5)	O6vi—Na1—Zn1	113.43 (6)
O7iv—Zn1—Na1	115.05 (6)	O1i—Na1—Zn1	89.37 (5)
O7—Zn1—Na1	64.95 (6)	C4i—Na1—Zn1	152.38 (6)
O5iv—Zn1—Na1iv	144.12 (5)	C8iv—Na1—Zn1	53.66 (5)
O5—Zn1—Na1iv	35.88 (5)	Na1i—Na1—Zn1	90.01 (4)
O3iv—Zn1—Na1iv	64.27 (5)	Na2—Na1—Zn1	133.42 (4)
O3—Zn1—Na1iv	115.73 (5)	O5iv—Na1—Na2ix	86.09 (5)
O7iv—Zn1—Na1iv	64.95 (6)	O1—Na1—Na2ix	150.32 (6)
O7—Zn1—Na1iv	115.05 (6)	O4i—Na1—Na2ix	40.74 (5)
Na1—Zn1—Na1iv	180.0	O6vi—Na1—Na2ix	79.96 (6)
O4v—Na2—O3i	100.76 (7)	O1i—Na1—Na2ix	93.45 (6)
O4v—Na2—O6vi	92.41 (7)	C4i—Na1—Na2ix	66.06 (6)
O3i—Na2—O6vi	98.70 (7)	C8iv—Na1—Na2ix	64.99 (5)
O4v—Na2—O2	132.94 (7)	Na1i—Na1—Na2ix	131.30 (6)
O3i—Na2—O2	125.58 (7)	Na2—Na1—Na2ix	101.14 (3)
O6vi—Na2—O2	88.62 (7)	Zn1—Na1—Na2ix	118.12 (3)
O4v—Na2—O2vii	86.70 (7)	C1—O1—Na1	134.25 (16)
O3i—Na2—O2vii	102.18 (7)	C1—O1—Na1i	133.31 (16)
O6vi—Na2—O2vii	158.90 (8)	Na1—O1—Na1i	86.09 (7)
O2—Na2—O2vii	76.80 (7)	C1—O1—Na2	92.17 (15)
O4v—Na2—O1	168.90 (7)	Na1—O1—Na2	85.84 (6)
O3i—Na2—O1	77.54 (7)	Na1i—O1—Na2	117.27 (8)
O6vi—Na2—O1	77.12 (7)	O1—C1—O2	123.1 (2)
O2—Na2—O1	51.60 (6)	O1—C1—C2	120.3 (2)
O2vii—Na2—O1	104.40 (7)	O2—C1—C2	116.6 (2)
O4v—Na2—Na1	125.09 (6)	Zn1—O7—H1	115 (2)
O3i—Na2—Na1	62.16 (5)	C3—O7—H1	108.9 (16)
O6vi—Na2—Na1	46.67 (5)	C1—C2—H2A	109
O2—Na2—Na1	87.87 (5)	C1—C2—H2B	109
O2vii—Na2—Na1	145.37 (6)	C3—C2—H2A	108
O1—Na2—Na1	44.35 (5)	C3—C2—H2B	109
O4v—Na2—Na1viii	40.79 (5)	H2A—C2—H2B	108
O3i—Na2—Na1viii	123.00 (6)	C3—C5—H5A	107
O6vi—Na2—Na1viii	57.61 (5)	C3—C5—H5B	108
O2—Na2—Na1viii	106.39 (6)	C8—C5—H5A	107
O2vii—Na2—Na1viii	111.68 (5)	C8—C5—H5B	108
O1—Na2—Na1viii	131.31 (6)	H5A—C5—H5B	107

D—H···A	D—H	H···A	D···A	D—H···A
O7—H1···O2x	0.95 (3)	1.69 (3)	2.635 (2)	174 (3)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H1⋯O2i	0.95 (3)	1.69 (3)	2.635 (2)	174 (3)

Symmetry code: (i) .