Poly[[μ₄-4-(carb­oxylato­meth­yl)benzoato]zinc(II)]

In the title compound, [Zn(C₉H₆O₄)]_n, the Zn^II cations are coordinated in a tetra­hedral fashion by carboxyl­ate O-atom donors belonging to four 4-(carb­oxy­meth­yl) benzoate (4-cmb) ligands. Each 4-cmb ligand binds to four Zn^II cations in an exo­tetra­dentate fashion to create a non-inter­penetrated [Zn(4-cmb)]_n three-dimensional coordination polymer network with a new non-diamondoid 6⁶ topology. The crystal studied was refined as an inversion twin.

checkCIF/PLATON results

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Datablock: I


Alert level B
PLAT090_ALERT_3_B Poor Data / Parameter Ratio (Zmax > 18) ........       5.98 Note

Alert level C
STRVA01_ALERT_4_C           Flack test results are ambiguous.
           From the CIF: _refine_ls_abs_structure_Flack    0.440
           From the CIF: _refine_ls_abs_structure_Flack_su    0.019

Alert level G
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          3 Info
PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.18 Ratio
PLAT794_ALERT_5_G Tentative Bond Valency for Zn1       (II)      .       2.00 Info
PLAT802_ALERT_4_G CIF Input Record(s) with more than 80 Characters         14 Info
PLAT961_ALERT_5_G Dataset Contains no Negative Intensities .......     Please Check
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          5 Info

   0 ALERT level A = Most likely a serious problem - resolve or explain
   1 ALERT level B = A potentially serious problem, consider carefully
   1 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   6 ALERT level G = General information/check it is not something unexpected

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion
   3 ALERT type 5 Informative message, check

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Computing details

Data collection: COSMO (Bruker, 2013); cell refinement: SAINT (Bruker, 2013); data reduction: SAINT (Bruker, 2013); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL (Sheldrick, 2015); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Poly[[µ₄-4-(carboxylatomethyl)benzoato]zinc(II)]

Crystal data

[Zn(C9H6O4)]	Dx = 2.000 Mg m^−3
Mr = 243.51	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pca21	Cell parameters from 4707 reflections
a = 9.6314 (11) Å	θ = 2.4–25.4°
b = 4.8612 (6) Å	µ = 3.02 mm^−1
c = 17.269 (2) Å	T = 173 K
V = 808.54 (17) Å^3	Block, colorless
Z = 4	0.11 × 0.07 × 0.05 mm
F(000) = 488

Data collection

Bruker APEXII CCD diffractometer	1474 independent reflections
Radiation source: sealed tube	1441 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.026
Detector resolution: 8.36 pixels mm^-1	θmax = 25.4°, θmin = 2.4°
ω scans	h = −11→11
Absorption correction: multi-scan (SADABS; Bruker, 2013)	k = −5→5
Tmin = 0.608, Tmax = 0.745	l = −20→20
5902 measured reflections

Refinement

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.019	w = 1/[σ^2(Fo^2) + (0.0274P)^2 + 0.2338P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.049	(Δ/σ)max < 0.001
S = 1.07	Δρmax = 0.41 e Å^−3
1474 reflections	Δρmin = −0.26 e Å^−3
128 parameters	Absolute structure: Refined as an inversion twin
1 restraint	Absolute structure parameter: 0.440 (19)
Primary atom site location: dual

Special details

Experimental. Data was collected using a BRUKER CCD (charge coupled device) based diffractometer equipped with an Oxford low-temperature apparatus operating at 173 K. A suitable crystal was chosen and mounted on a nylon loop using Paratone oil. Data were measured using omega scans of 0.5° per frame for 30 s. The total number of images were based on results from the program COSMO where redundancy was expected to be 4 and completeness to 0.83Å to 100%. Cell parameters were retrieved using APEX II software and refined using SAINT on all observed reflections.Data reduction was performed using the SAINT software which corrects for Lp. Scaling and absorption corrections were applied using SADABS6 multi-scan technique, supplied by George Sheldrick. The structure was solved by the direct method using the SHELXT program and refined by least squares method on F2, SHELXL, incorporated in OLEX2.

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.

Refinement. The structure was refined by Least Squares using version 2018/3 of XL (Sheldrick, 2015) incorporated in Olex2 (Dolomanov et al., 2009). All non-hydrogen atoms were refined anisotropically. Hydrogen atom positions were calculated geometrically and refined using the riding model.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.56331 (4)	0.57814 (7)	0.73682 (2)	0.01480 (14)
O3	−0.0109 (3)	0.3545 (6)	0.32739 (16)	0.0183 (6)
O2	0.2616 (3)	0.4478 (5)	0.71219 (15)	0.0190 (7)
O4	−0.0524 (3)	−0.0286 (6)	0.26387 (17)	0.0209 (7)
O1	0.4561 (3)	0.4858 (7)	0.64554 (17)	0.0198 (6)
C2	0.2647 (4)	0.3138 (8)	0.5782 (2)	0.0171 (8)
C5	0.1557 (4)	0.0862 (7)	0.4423 (2)	0.0170 (8)
C1	0.3286 (4)	0.4242 (7)	0.6498 (2)	0.0145 (8)
C6	0.2485 (4)	0.3057 (8)	0.4389 (3)	0.0191 (8)
H6	0.2738	0.3798	0.3900	0.023*
C8	0.1057 (5)	−0.0552 (8)	0.3698 (3)	0.0203 (9)
H8A	0.0600	−0.2290	0.3853	0.024*
H8B	0.1883	−0.1051	0.3387	0.024*
C7	0.3041 (4)	0.4171 (7)	0.5055 (2)	0.0167 (8)
H7	0.3691	0.5638	0.5022	0.020*
C4	0.1169 (4)	−0.0147 (8)	0.5143 (3)	0.0190 (8)
H4	0.0531	−0.1634	0.5173	0.023*
C9	0.0067 (4)	0.0996 (8)	0.3177 (2)	0.0161 (8)
C3	0.1700 (4)	0.0985 (7)	0.5818 (2)	0.0171 (8)
H3	0.1415	0.0287	0.6307	0.021*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0149 (2)	0.0164 (2)	0.0131 (2)	−0.00133 (14)	0.0010 (2)	−0.0021 (2)
O3	0.0217 (16)	0.0151 (13)	0.0181 (14)	0.0020 (12)	−0.0014 (13)	0.0002 (11)
O2	0.0129 (13)	0.0284 (15)	0.0156 (15)	0.0007 (10)	0.0007 (10)	−0.0013 (11)
O4	0.0286 (17)	0.0157 (13)	0.0185 (15)	0.0017 (11)	−0.0095 (11)	−0.0052 (11)
O1	0.0168 (15)	0.0291 (15)	0.0136 (15)	−0.0051 (13)	−0.0003 (12)	−0.0045 (14)
C2	0.015 (2)	0.0170 (19)	0.020 (2)	0.0027 (15)	0.0009 (16)	−0.0022 (17)
C5	0.0162 (19)	0.0146 (19)	0.020 (2)	0.0057 (14)	−0.0049 (18)	−0.0007 (16)
C1	0.013 (2)	0.0136 (19)	0.016 (2)	−0.0007 (14)	−0.0022 (16)	0.0023 (15)
C6	0.023 (2)	0.018 (2)	0.016 (2)	−0.0001 (18)	0.0031 (18)	0.0010 (17)
C8	0.025 (2)	0.016 (2)	0.020 (2)	0.0022 (16)	−0.0039 (19)	−0.0017 (17)
C7	0.016 (2)	0.0153 (19)	0.019 (2)	−0.0009 (14)	0.0013 (15)	−0.0004 (16)
C4	0.016 (2)	0.0178 (18)	0.023 (2)	−0.0030 (16)	−0.0008 (17)	−0.0028 (17)
C9	0.016 (2)	0.019 (2)	0.0134 (19)	−0.0016 (15)	0.0025 (16)	−0.0009 (15)
C3	0.017 (2)	0.0184 (19)	0.016 (2)	−0.0002 (15)	0.0021 (16)	0.0020 (16)

Geometric parameters (Å, º)

Zn1—O3^i	1.971 (3)	C2—C3	1.390 (6)
Zn1—O2^ii	1.961 (3)	C5—C6	1.393 (5)
Zn1—O4^iii	1.971 (3)	C5—C8	1.507 (6)
Zn1—O1	1.937 (3)	C5—C4	1.387 (6)
O3—Zn1^iv	1.971 (3)	C6—H6	0.9500
O3—C9	1.261 (5)	C6—C7	1.379 (6)
O2—Zn1^v	1.961 (3)	C8—H8A	0.9900
O2—C1	1.262 (5)	C8—H8B	0.9900
O4—Zn1^vi	1.971 (3)	C8—C9	1.511 (6)
O4—C9	1.256 (5)	C7—H7	0.9500
O1—C1	1.266 (5)	C4—H4	0.9500
C2—C1	1.482 (6)	C4—C3	1.388 (6)
C2—C7	1.404 (6)	C3—H3	0.9500
O3^i—Zn1—O4^iii	109.47 (12)	C7—C6—C5	121.0 (4)
O2^ii—Zn1—O3^i	112.72 (12)	C7—C6—H6	119.5
O2^ii—Zn1—O4^iii	99.55 (11)	C5—C8—H8A	107.8
O1—Zn1—O3^i	112.43 (12)	C5—C8—H8B	107.8
O1—Zn1—O2^ii	109.13 (11)	C5—C8—C9	117.9 (3)
O1—Zn1—O4^iii	112.90 (14)	H8A—C8—H8B	107.2
C9—O3—Zn1^iv	118.1 (3)	C9—C8—H8A	107.8
C1—O2—Zn1^v	132.7 (3)	C9—C8—H8B	107.8
C9—O4—Zn1^vi	132.9 (3)	C2—C7—H7	120.0
C1—O1—Zn1	121.7 (3)	C6—C7—C2	120.0 (4)
C7—C2—C1	120.3 (3)	C6—C7—H7	120.0
C3—C2—C1	120.5 (4)	C5—C4—H4	119.5
C3—C2—C7	119.2 (4)	C5—C4—C3	120.9 (4)
C6—C5—C8	121.3 (4)	C3—C4—H4	119.5
C4—C5—C6	118.8 (4)	O3—C9—C8	119.7 (4)
C4—C5—C8	119.8 (3)	O4—C9—O3	121.6 (4)
O2—C1—O1	121.6 (4)	O4—C9—C8	118.6 (3)
O2—C1—C2	122.2 (3)	C2—C3—H3	119.9
O1—C1—C2	116.1 (4)	C4—C3—C2	120.1 (4)
C5—C6—H6	119.5	C4—C3—H3	119.9
Zn1^iv—O3—C9—O4	−25.6 (5)	C1—C2—C3—C4	−176.1 (4)
Zn1^iv—O3—C9—C8	151.8 (3)	C6—C5—C8—C9	−71.1 (5)
Zn1^v—O2—C1—O1	170.3 (3)	C6—C5—C4—C3	−0.5 (6)
Zn1^v—O2—C1—C2	−12.0 (5)	C8—C5—C6—C7	−173.7 (4)
Zn1^vi—O4—C9—O3	−173.7 (3)	C8—C5—C4—C3	175.0 (4)
Zn1^vi—O4—C9—C8	8.9 (6)	C7—C2—C1—O2	145.3 (4)
Zn1—O1—C1—O2	7.6 (5)	C7—C2—C1—O1	−36.9 (5)
Zn1—O1—C1—C2	−170.3 (3)	C7—C2—C3—C4	1.0 (6)
C5—C6—C7—C2	−1.6 (6)	C4—C5—C6—C7	1.7 (6)
C5—C8—C9—O3	13.3 (6)	C4—C5—C8—C9	113.6 (4)
C5—C8—C9—O4	−169.2 (4)	C3—C2—C1—O2	−37.7 (5)
C5—C4—C3—C2	−0.8 (6)	C3—C2—C1—O1	140.2 (4)
C1—C2—C7—C6	177.3 (4)	C3—C2—C7—C6	0.2 (6)

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