catena-Poly­[[di­aqua­zinc(II)-μ-benzene-1,3-dioxy­acetate] dihydrate]

The title coordination polymer, {[Zn(C₁₀H₈O₆)(H₂O)₂]·2H₂O}_n, was synthesized and characterized by X-ray crystallography. The crystal structure reveals the asymmetric unit to consist of the zinc(II) complex [Zn(1,3-BDOA)(H₂O)₂] and two uncoordinated water mol­ecules. The zinc(II) ion displays a four-coordinate distorted tetrahedral geometry, formed by two carboxyl­ate O atoms of two benzene-1,3-dioxy­acetate ligands and two coordinated water mol­ecules. The zinc(II) ions are bridged by carboxyl­ate groups, forming a one-dimensional chain structure. The Zn—O bond distances lie in the range 1.941 (4)–1.981 (4) Å and the Zn...Zn separation within the polymer is 14.627 (3) Å.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.009 Å
• H-atom completeness 51%
• R factor = 0.038
• wR factor = 0.093
• Data-to-parameter ratio = 9.2

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O3W
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O4W

Alert level B
PLAT430_ALERT_2_B Short Inter D...A Contact  O1W    ..  O4W      =       2.68 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O2W    ..  O3W      =       2.64 Ang.

Alert level C
CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.99 <> 1.01
           From the CIF: _cell_formula_units_Z                    4
           From the CIF: _chemical_formula_weight           361.60
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   10.00  120.11
           H         1.01    8.00    8.06
           O        16.00   10.00  159.99
           Zn       65.39    1.00   65.39
           Calculated formula weight              353.55
REFNR01_ALERT_3_C  Ratio of reflections to parameters is < 10 for a
            non-centrosymmetric structure, where ZMAX > 18
            sine(theta)/lambda                0.6492
            Proportion of unique data used    0.9203
            Ratio reflections to parameters   9.1737
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT043_ALERT_1_C Check Reported Molecular Weight ................     361.60
PLAT044_ALERT_1_C Calculated and Reported Dx Differ ..............          ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       3.69
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....         O3
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....         O4
PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor ....       2.18
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          9
PLAT430_ALERT_2_C Short Inter D...A Contact  O3W    ..  O6       =       2.87 Ang.
PLAT430_ALERT_2_C Short Inter D...A Contact  O4W    ..  O6       =       2.85 Ang.
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............          !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............          !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............          !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............          !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............          !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............          !

Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C10 H16 O10 Zn1
            Atom count from the _atom_site data:  C10 H8 O10 Zn1
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    4
           From the CIF: _chemical_formula_sum  C10 H16 O10 Zn
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C         40.00     40.00    0.00
           H         64.00     32.00   32.00
           O         40.00     40.00    0.00
           Zn         4.00      4.00    0.00
REFLT03_ALERT_4_G  WARNING: Large fraction of Friedel related reflns may
                     be needed to determine absolute structure
           From the CIF: _diffrn_reflns_theta_max           27.48
           From the CIF: _reflns_number_total               1894
           Count of symmetry unique reflns         1749
           Completeness (_total/calc)            108.29%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured       145
           Fraction of Friedel pairs measured     0.083
           Are heavy atom types Z>Si present          yes

   2 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
  20 ALERT level C = Check and explain
   4 ALERT level G = General alerts; check

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

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Computing details

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); 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.

catena-Poly[[diaquazinc(II)-µ-benzene-1,3-dioxyacetate] dihydrate]

Crystal data

[Zn(C10H8O6)(H2O)2]·2H2O	Dx = 1.731 Mg m^−3
Mr = 361.60	Melting point: not measured K
Orthorhombic, Pna21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2n	Cell parameters from 12865 reflections
a = 8.604 (2) Å	θ = 3.5–27.4°
b = 27.271 (6) Å	µ = 1.82 mm^−1
c = 5.914 (1) Å	T = 293 K
V = 1387.7 (5) Å^3	Sheet, colorless
Z = 4	0.24 × 0.14 × 0.08 mm
F(000) = 744

Data collection

Rigaku R-AXIS RAPID diffractometer	1894 independent reflections
Radiation source: fine-focus sealed tube	1329 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.044
Detector resolution: 10.000 pixels mm^-1	θmax = 27.5°, θmin = 3.3°
ω scans	h = 0→11
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = 0→35
Tmin = 0.669, Tmax = 0.868	l = 0→7
13514 measured reflections

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)] = 0.038	H-atom parameters constrained
wR(F^2) = 0.093	w = 1/[σ^2(Fo^2) + (0.0591P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.92	(Δ/σ)max = 0.001
1743 reflections	Δρmax = 1.15 e Å^−3
190 parameters	Δρmin = −0.31 e Å^−3
1 restraint	Absolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.07 (3)

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	0.33986 (7)	0.595051 (17)	0.21902 (16)	0.03328 (17)
O1	0.4292 (5)	0.64105 (13)	0.4354 (7)	0.0365 (10)
O2	0.5326 (5)	0.57999 (13)	0.6328 (7)	0.0401 (10)
O3	0.6805 (5)	0.64030 (13)	0.9048 (8)	0.0462 (12)
O4	1.0172 (5)	0.64130 (13)	1.5185 (7)	0.0488 (12)
O5	1.2569 (5)	0.64131 (13)	2.0007 (7)	0.0346 (9)
O6	1.1441 (4)	0.58064 (13)	1.8075 (7)	0.0392 (10)
O1W	0.1770 (5)	0.55237 (14)	0.3504 (8)	0.0455 (11)
O2W	0.4861 (5)	0.54992 (13)	0.0791 (8)	0.0463 (11)
O3W	0.7430 (6)	0.51800 (14)	0.2754 (9)	0.0612 (14)
O4W	0.1595 (4)	0.45763 (12)	0.2333 (15)	0.0527 (10)
C1	0.5126 (6)	0.62376 (19)	0.5932 (9)	0.0314 (12)
C2	0.5891 (6)	0.66310 (17)	0.7405 (14)	0.0293 (11)
H2A	0.6531	0.6843	0.6475	0.035*
H2B	0.5098	0.6830	0.8124	0.035*
C3	0.7584 (6)	0.66886 (19)	1.0566 (10)	0.0281 (12)
C4	0.7537 (6)	0.71957 (18)	1.0605 (10)	0.0346 (13)
H4	0.6936	0.7367	0.9563	0.042*
C5	0.8400 (6)	0.74457 (15)	1.2225 (18)	0.0379 (10)
H5	0.8370	0.7787	1.2250	0.045*
C6	0.9289 (6)	0.72054 (18)	1.3773 (11)	0.0336 (13)
H6	0.9856	0.7379	1.4847	0.040*
C7	0.9331 (6)	0.66971 (19)	1.3717 (10)	0.0308 (12)
C8	0.8491 (6)	0.64395 (15)	1.2104 (16)	0.0302 (10)
H8A	0.8540	0.6099	1.2061	0.036*
C9	1.0997 (6)	0.66450 (17)	1.6983 (13)	0.0299 (13)
H9A	1.0295	0.6846	1.7871	0.036*
H9B	1.1808	0.6854	1.6377	0.036*
C10	1.1700 (6)	0.62504 (18)	1.8444 (9)	0.0276 (11)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0433 (3)	0.0303 (2)	0.0262 (2)	−0.0025 (3)	−0.0106 (4)	0.0015 (5)
O1	0.045 (2)	0.035 (2)	0.030 (2)	−0.0026 (18)	−0.020 (2)	0.002 (2)
O2	0.049 (2)	0.0308 (17)	0.041 (2)	0.0043 (18)	−0.017 (2)	−0.0034 (18)
O3	0.062 (3)	0.0276 (18)	0.049 (3)	0.0016 (19)	−0.042 (3)	−0.002 (2)
O4	0.070 (3)	0.0308 (18)	0.046 (3)	0.007 (2)	−0.043 (3)	−0.006 (2)
O5	0.039 (2)	0.0360 (19)	0.029 (2)	−0.0052 (19)	−0.017 (2)	0.003 (2)
O6	0.047 (2)	0.0302 (16)	0.040 (2)	−0.0001 (18)	−0.017 (2)	0.0006 (17)
O1W	0.056 (3)	0.041 (2)	0.040 (2)	−0.012 (2)	0.013 (2)	−0.005 (2)
O2W	0.046 (2)	0.042 (2)	0.051 (3)	0.006 (2)	0.003 (2)	0.003 (2)
O3W	0.074 (3)	0.048 (2)	0.061 (4)	0.017 (2)	−0.004 (3)	0.010 (2)
O4W	0.0424 (19)	0.0421 (17)	0.074 (3)	−0.0017 (18)	−0.001 (3)	−0.005 (4)
C1	0.025 (3)	0.043 (3)	0.026 (3)	−0.002 (2)	−0.003 (3)	−0.004 (3)
C2	0.031 (2)	0.031 (2)	0.026 (3)	−0.0001 (19)	−0.012 (3)	0.002 (3)
C3	0.028 (3)	0.027 (2)	0.029 (3)	0.001 (2)	−0.013 (3)	−0.001 (2)
C4	0.036 (3)	0.031 (3)	0.037 (3)	0.003 (2)	−0.015 (3)	0.004 (3)
C5	0.045 (3)	0.0244 (18)	0.044 (2)	0.001 (2)	−0.012 (4)	−0.007 (5)
C6	0.042 (3)	0.026 (2)	0.033 (3)	−0.007 (2)	−0.012 (3)	−0.006 (2)
C7	0.033 (3)	0.032 (2)	0.027 (3)	0.003 (2)	−0.010 (3)	0.005 (2)
C8	0.037 (2)	0.0237 (17)	0.030 (2)	0.000 (2)	−0.011 (3)	−0.008 (4)
C9	0.031 (2)	0.029 (2)	0.029 (3)	0.0026 (19)	−0.014 (3)	−0.006 (3)
C10	0.025 (3)	0.036 (3)	0.022 (3)	0.000 (2)	−0.005 (3)	0.001 (2)

Geometric parameters (Å, º)

Zn1—O5^i	1.941 (4)	C2—H2B	0.9700
Zn1—O2W	1.945 (4)	C3—C8	1.377 (9)
Zn1—O1	1.950 (4)	C3—C4	1.384 (7)
Zn1—O1W	1.981 (4)	C4—C5	1.391 (9)
O1—C1	1.268 (6)	C4—H4	0.9300
O2—C1	1.228 (6)	C5—C6	1.361 (10)
O3—C3	1.364 (6)	C5—H5	0.9300
O3—C2	1.397 (8)	C6—C7	1.387 (7)
O4—C7	1.370 (6)	C6—H6	0.9300
O4—C9	1.427 (7)	C7—C8	1.388 (9)
O5—C10	1.269 (6)	C8—H8A	0.9300
O5—Zn1^ii	1.941 (4)	C9—C10	1.507 (8)
O6—C10	1.250 (6)	C9—H9A	0.9700
C1—C2	1.531 (8)	C9—H9B	0.9700
C2—H2A	0.9700
O5^i—Zn1—O2W	111.5 (2)	C3—C4—H4	120.5
O5^i—Zn1—O1	99.4 (1)	C5—C4—H4	120.5
O2W—Zn1—O1	115.5 (2)	C6—C5—C4	121.8 (4)
O5^i—Zn1—O1W	112.5 (2)	C6—C5—H5	119.1
O2W—Zn1—O1W	104.7 (2)	C4—C5—H5	119.1
O1—Zn1—O1W	113.6 (2)	C5—C6—C7	118.7 (5)
C1—O1—Zn1	117.8 (3)	C5—C6—H6	120.7
C3—O3—C2	118.7 (4)	C7—C6—H6	120.7
C7—O4—C9	119.0 (4)	O4—C7—C6	124.3 (5)
C10—O5—Zn1^ii	118.3 (3)	O4—C7—C8	115.1 (5)
O2—C1—O1	125.5 (5)	C6—C7—C8	120.5 (5)
O2—C1—C2	120.8 (5)	C3—C8—C7	120.0 (4)
O1—C1—C2	113.7 (4)	C3—C8—H8A	120.0
O3—C2—C1	109.0 (4)	C7—C8—H8A	120.0
O3—C2—H2A	109.9	O4—C9—C10	108.1 (4)
C1—C2—H2A	109.9	O4—C9—H9A	110.1
O3—C2—H2B	109.9	C10—C9—H9A	110.1
C1—C2—H2B	109.9	O4—C9—H9B	110.1
H2A—C2—H2B	108.3	C10—C9—H9B	110.1
O3—C3—C8	115.5 (5)	H9A—C9—H9B	108.4
O3—C3—C4	124.5 (5)	O6—C10—O5	124.8 (5)
C8—C3—C4	119.9 (5)	O6—C10—C9	121.3 (5)
C3—C4—C5	119.1 (5)	O5—C10—C9	113.8 (4)
O5^i—Zn1—O1—C1	−171.5 (4)	C9—O4—C7—C6	3.7 (9)
O2W—Zn1—O1—C1	−52.2 (5)	C9—O4—C7—C8	−176.3 (6)
O1W—Zn1—O1—C1	68.8 (4)	C5—C6—C7—O4	−179.7 (6)
Zn1—O1—C1—O2	−6.1 (8)	C5—C6—C7—C8	0.4 (10)
Zn1—O1—C1—C2	174.7 (4)	O3—C3—C8—C7	179.9 (6)
C3—O3—C2—C1	−179.4 (5)	C4—C3—C8—C7	1.3 (10)
O2—C1—C2—O3	2.1 (8)	O4—C7—C8—C3	178.9 (5)
O1—C1—C2—O3	−178.7 (5)	C6—C7—C8—C3	−1.1 (10)
C2—O3—C3—C8	−178.5 (6)	C7—O4—C9—C10	175.2 (5)
C2—O3—C3—C4	0.0 (9)	Zn1^ii—O5—C10—O6	−6.6 (8)
O3—C3—C4—C5	−179.2 (6)	Zn1^ii—O5—C10—C9	174.4 (4)
C8—C3—C4—C5	−0.7 (9)	O4—C9—C10—O6	−4.3 (8)
C3—C4—C5—C6	−0.1 (11)	O4—C9—C10—O5	174.7 (4)
C4—C5—C6—C7	0.2 (11)

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