Poly[tetra­kis(μ-cyclo­hexa­ne-1,4-di­carboxyl­ato)di-μ-hydroxido-penta­zinc(II)]

Chen, J.-X.; Meng, W.-W.

doi:10.1107/S1600536809051666

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 1| January 2010| Pages m16-m17

doi:10.1107/S1600536809051666

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Poly[tetrakis(μ-cyclohexane-1,4-dicarboxylato)di-μ-hydroxido-pentazinc(II)]

Jin-Xi Chen ^a ^* and Wei-Wei Meng ^a

^aSchool of Chemistry and Chemical Engineering, Southeast University, Nanjing 211189, People's Republic of China
^*Correspondence e-mail: mww_514730@yahoo.com.cn

(Received 8 November 2009; accepted 1 December 2009; online 4 December 2009)

In the title coordination polymer, [Zn₅(μ₃-OH)₂(1,4-CDC)₄]_n (1,4-CDCH₂ = 1,4-cyclohexanedicarboxylic acid) or [Zn₅(C₈H₁₀O₄)₄(OH)₂]_n, the asymmetric unit comprises one half of an octahedrally coordinated ZnO₆ complex unit (site symmetry $[\overline1]$ ) and two five-coordinate ZnO₅ complex units, together with two μ₃-bridging hydroxido ligands and four 1,4-CDC ligands (comprising two whole molecules and four inversion-related half-molecules). The ZnO₆ unit consists of four carboxylate O donors (two bridging) and two hydroxido O donors (both bridging three Zn centres) [Zn—O range 2.065 (3)–2.125 (3) Å]. Each of the ZnO₅ units [one capped tetrahedral, the other square-pyrimidal; Zn—O range 1.928 (3)–2.338 (3) Å] has one hydroxido O donor and four carboxyl O donors from three different 1,4-CDC carboxylate O donors (one bridging). Infinite (ZnO)_n inorganic chains run parallel to the a axis and are interconnected by the organic ligands into a three-dimensional structure.

Related literature

For the structures of related complexes of 1,4-cyclohexanedicarboxylic acid, see: Liu, Huang et al. (2009 ); Liu, Zhu et al. (2009 ); Yang et al. (2007 ); Du et al. (2005 ).

Experimental

Crystal data

[Zn₅(C₈H₁₀O₄)₄(OH)₂]
M_r = 1039.59
Triclinic, $[P \overline 1]$
a = 8.646 (3) Å
b = 10.665 (3) Å
c = 11.804 (3) Å
α = 113.915 (3)°
β = 96.307 (3)°
γ = 106.285 (3)°
V = 923.6 (5) Å³
Z = 1
Mo Kα radiation
μ = 3.28 mm⁻¹
T = 295 K
0.20 × 0.20 × 0.20 mm

Data collection

Rigaku SCXmini diffractometer
3929 measured reflections
3202 independent reflections
2789 reflections with I > 2σ(I)
R_int = 0.019

Refinement

R[F² > 2σ(F²)] = 0.038
wR(F²) = 0.095
S = 1.04
3202 reflections
250 parameters
H-atom parameters constrained
Δρ_max = 1.11 e Å⁻³
Δρ_min = −0.50 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: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, New_Global_Publ_Block. DOI: 10.1107/S1600536809051666/zs2020sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809051666/zs2020Isup2.hkl

checkCIF report

Comment top

In recent years, new coordination compounds formed from reaction of metals with cyclohexane-1,4-dicarboxylic acid [1,4-CDCH₂] have attracted much attention (Liu, Huang et al., 2009; Liu, Zhu et al., 2009; Yang et al., 2007; Du et al., 2005). The structure of the title complex from the reaction of this acid with Zn^II ion, [Zn₅(µ₃-OH)₂(1,4-CDC)₄]_n (I) has been determined and the structure is reported here.

Compound (I) is a coordination polymer in which the repeating unit lies on a crystallographic inversion centre,the asymmetric unit comprising a half of an octahedraly coordinated Zn atom (Zn1) which lies on the centre, two five-coordinate Zn atoms in (Zn2 and Zn3), general sites, one µ₃-hydroxido ligand (O1) and two cyclohexane-1,4-dicarboxylate ligands (Fig. 1). One of these 1,4-CDC ligands is complete (associated with donor atoms O6, O8, O3, O7) while the other 1,4-CDC ligand consists of two inversion-related halves (associated with O4, O5 and O2, O9). The ZnO₆ coordination sphere about Zn1 consists of four carboxylate O donors (two bridging) and two hydroxido O donors (both bridging three Zn centres), [Zn—O bond length range, 2.065 (3)–2.125 (3) Å]. Both Zn2 and Zn3 are five coordinate, Zn2 having a capped tetrahedral stereochemistry, comprising one bridging hydroxyl O donor and four O donors from three different 1,4-CDC ligands (one bridging) [Zn–O bond length and O–Zn–O bond angle ranges, 1.928 (3)–2.338 (3) Å and 58.85 (11)–145.39 (12)° respectively]. The stereochemistry about Zn3 is tetragonal pyramidal with the four basal coordination sites occupied by O donor atoms from three different 1,4-CDC ligands (one bridging) [Zn—O range, 1.938 (3)–2.207 (3) Å], with the axial site occupied by the bridging hydroxido O donor [Zn–O1, 1.977 (3) Å]. The bond angle range is 86.00 (12)–125.97 (12)°. The repeat units form infinite (ZnO)_n inorganic chains parallel to the a-axis which are interconnected by the organic ligands into a three-dimensional structure (Fig. 2).

Related literature top

For the structures of related complexes of cyclohexane-1,4-dicarboxylic acid, see: Liu, Huang et al. (2009); Liu, Zhu et al. (2009); Yang et al. (2007); Du et al. (2005). Scheme - the repeat unit inside the brackets should be two whole and four half cyclohexanedicarboxylate ligands instead of eight whole ones

Experimental top

An aqueous mixture of cyclohexane-1,4-dicarboxylic acid (0.086 g, 0.5 mmol) and NaOH (0.040 g, 1 mmol) in 8 ml of water was stirred for half an hour. The pH was adjusted to ca. 7 with 1M HNO₃ and (0.147 g, 0.5 mmol) of Zn(NO₃)₂ . 6H₂O was added and the solution was stirred for half an hour. After adding 3 ml of cyclohexanol, the mixture was transferred into a 23 ml Teflon-lined autoclave and heated at 180° for 120 h. After cooling to room temperature, colorless single crystal blocks were obtained, which were washed with water.

Computing details top

Data collection: CrystalClear (Rigaku, 2005); cell refinement: CrystalClear (Rigaku, 2005); data reduction: CrystalClear (Rigaku, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); 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. The asymmetric unit of the title compound (I), with displacement ellipsoids drawn at the 30% probability level. For symmetry codes: (A),-x+1,-y+1,-z+1; (B),-x,-y+1,-z+1; (C),-x,-y,-z; (D),-x,-y+2,-z+1; (E), -x,-y-1,-z+1;(F),-x+1,-y+1,-z; (G), x+1, y+1, z+1; (H), x, y,z+1.
	Fig. 2. The two-dimensional framework polymer structure of (I).

Poly[tetrakis(µ-cyclohexane-1,4-dicarboxylato)di-µ-hydroxido-pentazinc(II)] top

Crystal data top

[Zn₅(OH)₂(C₈H₁₀O₄)₄]	Z = 1
M_r = 1039.59	F(000) = 526
Triclinic, P1	D_x = 1.869 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.646 (3) Å	Cell parameters from 30 reflections
b = 10.665 (3) Å	θ = 3–25°
c = 11.804 (3) Å	µ = 3.28 mm⁻¹
α = 113.915 (3)°	T = 295 K
β = 96.307 (3)°	Block, colorless
γ = 106.285 (3)°	0.20 × 0.20 × 0.20 mm
V = 923.6 (5) Å³

Data collection top

Rigaku SCXmini diffractometer	R_int = 0.019
Radiation source: fine-focus sealed tube	θ_max = 25.0°, θ_min = 2.0°
Graphite monochromator	h = −10→10
ω scans	k = −12→9
3929 measured reflections	l = −14→13
3202 independent reflections	3 standard reflections every 150 reflections
2789 reflections with I > 2σ(I)	intensity decay: none

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)] = 0.038	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.095	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0488P)² + 2.2254P] where P = (F_o² + 2F_c²)/3
3202 reflections	(Δ/σ)_max < 0.001
250 parameters	Δρ_max = 1.11 e Å⁻³
0 restraints	Δρ_min = −0.50 e Å⁻³

Crystal data top

[Zn₅(OH)₂(C₈H₁₀O₄)₄]	γ = 106.285 (3)°
M_r = 1039.59	V = 923.6 (5) Å³
Triclinic, P1	Z = 1
a = 8.646 (3) Å	Mo Kα radiation
b = 10.665 (3) Å	µ = 3.28 mm⁻¹
c = 11.804 (3) Å	T = 295 K
α = 113.915 (3)°	0.20 × 0.20 × 0.20 mm
β = 96.307 (3)°

Data collection top

Rigaku SCXmini diffractometer	R_int = 0.019
3929 measured reflections	3 standard reflections every 150 reflections
3202 independent reflections	intensity decay: none
2789 reflections with I > 2σ(I)

Refinement top

R[F² > 2σ(F²)] = 0.038	0 restraints
wR(F²) = 0.095	H-atom parameters constrained
S = 1.04	Δρ_max = 1.11 e Å⁻³
3202 reflections	Δρ_min = −0.50 e Å⁻³
250 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
Zn1	0.5000	0.5000	0.5000	0.01886 (17)
Zn2	0.23318 (6)	0.53614 (5)	0.33384 (4)	0.02004 (14)
Zn3	0.22931 (6)	0.63639 (5)	0.63471 (4)	0.02095 (15)
O1	0.2545 (3)	0.4858 (3)	0.4786 (2)	0.0165 (6)
O2	0.4649 (3)	0.5325 (3)	0.3351 (3)	0.0227 (6)
O3	−0.0494 (4)	0.3940 (3)	0.2794 (3)	0.0260 (7)
O4	0.0760 (4)	0.7048 (3)	0.5332 (3)	0.0292 (7)
O5	0.2146 (4)	0.7268 (3)	0.3889 (3)	0.0329 (8)
O6	0.4102 (4)	0.2695 (3)	0.3800 (3)	0.0333 (8)
O7	0.1035 (4)	0.4072 (4)	0.1489 (3)	0.0354 (8)
O8	0.5888 (4)	0.1755 (3)	0.2861 (3)	0.0367 (8)
O9	0.6515 (4)	0.4466 (4)	0.2502 (3)	0.0391 (9)
C1	−0.0356 (5)	0.3514 (5)	0.1658 (4)	0.0216 (9)
C2	0.4892 (6)	0.5179 (5)	0.1295 (4)	0.0244 (9)
H2	0.4089	0.5681	0.1453	0.029*
C3	0.5402 (5)	0.4959 (5)	0.2450 (4)	0.0210 (9)
C4	−0.1756 (5)	0.2307 (5)	0.0558 (4)	0.0239 (9)
H4	−0.2808	0.2294	0.0799	0.029*
C5	0.4451 (6)	0.1700 (5)	0.2982 (4)	0.0266 (10)
C6	0.3284 (6)	−0.1108 (5)	0.1772 (4)	0.0340 (11)
H6A	0.3326	−0.1206	0.2556	0.041*
H6B	0.4337	−0.1087	0.1553	0.041*
C7	0.4060 (6)	0.3693 (5)	0.0104 (4)	0.0293 (10)
H7A	0.4817	0.3156	−0.0022	0.035*
H7B	0.3068	0.3126	0.0236	0.035*
C8	0.3027 (5)	0.0317 (5)	0.1984 (4)	0.0274 (10)
H8	0.1995	0.0306	0.2258	0.033*
C9	0.6414 (6)	0.6136 (5)	0.1087 (4)	0.0330 (11)
H9A	0.6883	0.7096	0.1827	0.040*
H9B	0.7258	0.5689	0.1000	0.040*
C10	−0.1861 (6)	0.2424 (5)	−0.0691 (4)	0.0330 (11)
H10A	−0.0815	0.2467	−0.0928	0.040*
H10B	−0.2041	0.3323	−0.0568	0.040*
C11	0.1180 (6)	0.7593 (5)	0.4592 (4)	0.0281 (10)
C12	0.0494 (7)	0.8716 (6)	0.4494 (6)	0.0441 (13)
H12	0.0263	0.8499	0.3590	0.053*
C13	−0.1518 (7)	0.0883 (5)	0.0363 (5)	0.0425 (13)
H13A	−0.1540	0.0779	0.1141	0.051*
H13B	−0.0434	0.0922	0.0200	0.051*
C14	0.2867 (7)	0.0456 (5)	0.0755 (5)	0.0396 (12)
H14A	0.3928	0.0582	0.0533	0.047*
H14B	0.2606	0.1326	0.0894	0.047*
C15	0.1774 (7)	1.0209 (7)	0.5214 (7)	0.0554 (16)
H15A	0.2750	1.0237	0.4876	0.066*
H15B	0.2105	1.0432	0.6107	0.066*
C16	−0.1133 (7)	0.8624 (6)	0.4875 (7)	0.0518 (15)
H16A	−0.0976	0.8752	0.5746	0.062*
H16B	−0.1962	0.7657	0.4319	0.062*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn1	0.0198 (3)	0.0240 (4)	0.0140 (3)	0.0118 (3)	0.0024 (3)	0.0077 (3)
Zn2	0.0223 (3)	0.0226 (3)	0.0165 (3)	0.0107 (2)	0.00190 (19)	0.0092 (2)
Zn3	0.0198 (3)	0.0234 (3)	0.0170 (3)	0.0083 (2)	0.00536 (19)	0.0062 (2)
O1	0.0185 (13)	0.0181 (14)	0.0134 (13)	0.0092 (11)	0.0029 (11)	0.0062 (11)
O2	0.0255 (15)	0.0346 (17)	0.0163 (14)	0.0167 (13)	0.0072 (12)	0.0150 (13)
O3	0.0235 (15)	0.0329 (17)	0.0157 (15)	0.0074 (13)	0.0038 (12)	0.0077 (13)
O4	0.0330 (17)	0.0306 (17)	0.0320 (18)	0.0168 (14)	0.0109 (14)	0.0175 (15)
O5	0.0436 (19)	0.0259 (17)	0.045 (2)	0.0222 (15)	0.0220 (16)	0.0213 (15)
O6	0.0372 (19)	0.0199 (16)	0.0304 (18)	0.0063 (14)	0.0105 (15)	0.0020 (14)
O7	0.0249 (17)	0.046 (2)	0.0211 (17)	0.0037 (15)	0.0056 (13)	0.0077 (15)
O8	0.0246 (17)	0.0229 (17)	0.045 (2)	0.0037 (13)	0.0040 (15)	0.0030 (15)
O9	0.051 (2)	0.069 (2)	0.0274 (18)	0.046 (2)	0.0192 (16)	0.0314 (18)
C1	0.019 (2)	0.027 (2)	0.020 (2)	0.0133 (18)	0.0068 (17)	0.0076 (18)
C2	0.036 (2)	0.035 (3)	0.020 (2)	0.024 (2)	0.0138 (19)	0.020 (2)
C3	0.023 (2)	0.029 (2)	0.015 (2)	0.0126 (18)	0.0066 (16)	0.0118 (18)
C4	0.021 (2)	0.026 (2)	0.021 (2)	0.0091 (18)	0.0035 (17)	0.0071 (18)
C5	0.027 (2)	0.025 (2)	0.024 (2)	0.0082 (19)	0.0048 (18)	0.009 (2)
C6	0.047 (3)	0.026 (2)	0.017 (2)	0.005 (2)	−0.004 (2)	0.006 (2)
C7	0.033 (2)	0.032 (3)	0.028 (2)	0.011 (2)	0.0070 (19)	0.018 (2)
C8	0.023 (2)	0.023 (2)	0.025 (2)	0.0057 (18)	0.0033 (18)	0.0029 (19)
C9	0.036 (3)	0.037 (3)	0.024 (2)	0.009 (2)	0.002 (2)	0.017 (2)
C10	0.046 (3)	0.020 (2)	0.020 (2)	0.006 (2)	−0.002 (2)	0.0038 (19)
C11	0.030 (2)	0.024 (2)	0.033 (3)	0.0117 (19)	0.010 (2)	0.014 (2)
C12	0.062 (4)	0.038 (3)	0.059 (4)	0.033 (3)	0.034 (3)	0.032 (3)
C13	0.047 (3)	0.031 (3)	0.038 (3)	0.006 (2)	−0.011 (2)	0.016 (2)
C14	0.043 (3)	0.020 (2)	0.040 (3)	−0.001 (2)	−0.009 (2)	0.012 (2)
C15	0.042 (3)	0.056 (4)	0.084 (5)	0.029 (3)	0.019 (3)	0.038 (4)
C16	0.044 (3)	0.039 (3)	0.080 (4)	0.018 (3)	0.017 (3)	0.032 (3)

Geometric parameters (Å, º) top

Zn1—O1	2.065 (3)	C5—C8	1.528 (6)
Zn1—O1ⁱ	2.065 (3)	C6—C8	1.521 (6)
Zn1—O2ⁱ	2.116 (3)	C6—C10ⁱⁱⁱ	1.532 (6)
Zn1—O2	2.116 (3)	C6—H6A	0.9700
Zn1—O6	2.125 (3)	C6—H6B	0.9700
Zn1—O6ⁱ	2.125 (3)	C7—C9^iv	1.517 (6)
Zn2—O5	1.928 (3)	C7—H7A	0.9700
Zn2—O1	1.993 (3)	C7—H7B	0.9700
Zn2—O2	2.013 (3)	C8—C14	1.513 (7)
Zn2—O7	2.019 (3)	C8—H8	0.9800
Zn2—O3	2.338 (3)	C9—C7^iv	1.517 (6)
Zn3—O8ⁱ	1.939 (3)	C9—H9A	0.9700
Zn3—O3ⁱⁱ	1.971 (3)	C9—H9B	0.9700
Zn3—O1	1.977 (3)	C10—C6ⁱⁱⁱ	1.532 (6)
Zn3—O4	2.151 (3)	C10—H10A	0.9700
Zn3—O9ⁱ	2.207 (3)	C10—H10B	0.9700
O2—C3	1.290 (5)	C11—C12	1.516 (6)
O3—C1	1.261 (5)	C12—C15	1.480 (8)
O4—C11	1.263 (5)	C12—C16	1.513 (8)
O5—C11	1.260 (5)	C12—H12	0.9800
O6—C5	1.250 (5)	C13—C14ⁱⁱⁱ	1.530 (6)
O7—C1	1.261 (5)	C13—H13A	0.9700
O8—C5	1.254 (5)	C13—H13B	0.9700
O9—C3	1.226 (5)	C14—C13ⁱⁱⁱ	1.530 (6)
C1—C4	1.495 (6)	C14—H14A	0.9700
C2—C3	1.514 (5)	C14—H14B	0.9700
C2—C7	1.529 (6)	C15—C16^v	1.532 (7)
C2—C9	1.535 (6)	C15—H15A	0.9700
C2—H2	0.9800	C15—H15B	0.9700
C4—C13	1.518 (6)	C16—C15^v	1.532 (7)
C4—C10	1.524 (6)	C16—H16A	0.9700
C4—H4	0.9800	C16—H16B	0.9700

O1—Zn1—O2	80.38 (10)	O8—C5—C8	115.7 (4)
O1—Zn1—O6	87.49 (11)	C8—C6—C10ⁱⁱⁱ	110.4 (4)
O2—Zn1—O6	89.32 (12)	C8—C6—H6A	109.6
O1—Zn1—O6ⁱ	92.51 (11)	C10ⁱⁱⁱ—C6—H6A	109.6
O2—Zn1—O6ⁱ	90.68 (12)	C8—C6—H6B	109.6
O6—Zn1—O6ⁱ	180.00 (12)	C10ⁱⁱⁱ—C6—H6B	109.6
O1—Zn1—Zn2ⁱ	140.05 (7)	H6A—C6—H6B	108.1
O2—Zn1—Zn2ⁱ	139.33 (8)	C9^iv—C7—C2	111.9 (4)
O6—Zn1—Zn2ⁱ	88.74 (9)	C9^iv—C7—H7A	109.2
O5—Zn2—O1	111.19 (13)	C2—C7—H7A	109.2
O5—Zn2—O2	115.65 (13)	C9^iv—C7—H7B	109.2
O1—Zn2—O2	84.68 (11)	C2—C7—H7B	109.2
O5—Zn2—O7	108.81 (15)	H7A—C7—H7B	107.9
O1—Zn2—O7	129.58 (13)	C14—C8—C6	110.5 (4)
O2—Zn2—O7	104.36 (12)	C14—C8—C5	106.2 (4)
O5—Zn2—O3	98.81 (13)	C6—C8—C5	114.1 (4)
O1—Zn2—O3	85.57 (11)	C14—C8—H8	108.6
O2—Zn2—O3	145.41 (12)	C6—C8—H8	108.6
O7—Zn2—O3	58.86 (11)	C5—C8—H8	108.6
O8ⁱ—Zn3—O3ⁱⁱ	118.92 (13)	C7^iv—C9—C2	111.0 (4)
O8ⁱ—Zn3—O1	114.91 (13)	C7^iv—C9—H9A	109.4
O3ⁱⁱ—Zn3—O1	125.97 (12)	C2—C9—H9A	109.4
O8ⁱ—Zn3—O4	93.78 (14)	C7^iv—C9—H9B	109.4
O3ⁱⁱ—Zn3—O4	86.00 (12)	C2—C9—H9B	109.4
O1—Zn3—O4	94.98 (11)	H9A—C9—H9B	108.0
O8ⁱ—Zn3—O9ⁱ	92.49 (15)	C4—C10—C6ⁱⁱⁱ	111.1 (4)
O3ⁱⁱ—Zn3—O9ⁱ	84.37 (13)	C4—C10—H10A	109.4
O1—Zn3—O9ⁱ	89.19 (12)	C6ⁱⁱⁱ—C10—H10A	109.4
O4—Zn3—O9ⁱ	170.20 (13)	C4—C10—H10B	109.4
Zn3—O1—Zn2	111.16 (13)	C6ⁱⁱⁱ—C10—H10B	109.4
Zn3—O1—Zn1	110.07 (12)	H10A—C10—H10B	108.0
Zn2—O1—Zn1	98.36 (11)	O5—C11—O4	124.9 (4)
C3—O2—Zn2	132.3 (3)	O5—C11—C12	115.1 (4)
C3—O2—Zn1	125.5 (3)	O4—C11—C12	120.0 (4)
Zn2—O2—Zn1	96.09 (11)	C15—C12—C16	112.4 (5)
C1—O3—Zn3ⁱⁱ	137.0 (3)	C15—C12—C11	110.3 (5)
C1—O3—Zn2	84.3 (2)	C16—C12—C11	113.4 (4)
Zn3ⁱⁱ—O3—Zn2	138.63 (14)	C15—C12—H12	106.8
C11—O4—Zn3	125.9 (3)	C16—C12—H12	106.8
C11—O5—Zn2	118.8 (3)	C11—C12—H12	106.8
C5—O6—Zn1	142.7 (3)	C4—C13—C14ⁱⁱⁱ	112.1 (4)
C1—O7—Zn2	99.0 (3)	C4—C13—H13A	109.2
C5—O8—Zn3ⁱ	119.7 (3)	C14ⁱⁱⁱ—C13—H13A	109.2
C3—O9—Zn3ⁱ	140.7 (3)	C4—C13—H13B	109.2
O7—C1—O3	117.8 (4)	C14ⁱⁱⁱ—C13—H13B	109.2
O7—C1—C4	121.1 (4)	H13A—C13—H13B	107.9
O3—C1—C4	121.0 (4)	C8—C14—C13ⁱⁱⁱ	112.6 (4)
C3—C2—C7	110.1 (3)	C8—C14—H14A	109.1
C3—C2—C9	110.3 (4)	C13ⁱⁱⁱ—C14—H14A	109.1
C7—C2—C9	110.4 (4)	C8—C14—H14B	109.1
C3—C2—H2	108.6	C13ⁱⁱⁱ—C14—H14B	109.1
C7—C2—H2	108.6	H14A—C14—H14B	107.8
C9—C2—H2	108.6	C12—C15—C16^v	111.8 (5)
O9—C3—O2	122.9 (4)	C12—C15—H15A	109.2
O9—C3—C2	119.3 (4)	C16^v—C15—H15A	109.2
O2—C3—C2	117.8 (4)	C12—C15—H15B	109.2
C1—C4—C13	106.4 (4)	C16^v—C15—H15B	109.2
C1—C4—C10	115.0 (4)	H15A—C15—H15B	107.9
C13—C4—C10	109.7 (4)	C12—C16—C15^v	112.0 (5)
C1—C4—H4	108.5	C12—C16—H16A	109.2
C13—C4—H4	108.5	C15^v—C16—H16A	109.2
C10—C4—H4	108.5	C12—C16—H16B	109.2
O6—C5—O8	125.7 (4)	C15^v—C16—H16B	109.2
O6—C5—C8	118.6 (4)	H16A—C16—H16B	107.9

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

Experimental details

Crystal data
Chemical formula	[Zn₅(OH)₂(C₈H₁₀O₄)₄]
M_r	1039.59
Crystal system, space group	Triclinic, P1
Temperature (K)	295
a, b, c (Å)	8.646 (3), 10.665 (3), 11.804 (3)
α, β, γ (°)	113.915 (3), 96.307 (3), 106.285 (3)
V (Å³)	923.6 (5)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	3.28
Crystal size (mm)	0.20 × 0.20 × 0.20

Data collection
Diffractometer	Rigaku SCXmini diffractometer
Absorption correction	–
No. of measured, independent and observed [I > 2σ(I)] reflections	3929, 3202, 2789
R_int	0.019
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.038, 0.095, 1.04
No. of reflections	3202
No. of parameters	250
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.11, −0.50

Computer programs: CrystalClear (Rigaku, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Acknowledgements

We gratefully acknowledge financial support by the start-up fund of Southeast University.

References

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