catena-Poly[hexa­aqua­zinc(II) [bis­[dichloro­zincate(II)]-μ-pyridine-4-carboxyl­ato-κ²N,O] dihydrate]

In the title compound, {[ZnCl₂(C₆H₄NO₂)]₂[Zn(H₂O)₆]·2H₂O}_n, one Zn atom is involved in the formation of one-dimensional infinite zigzag anionic chains, whereas the second Zn atom, located on a twofold axis, is surrounded by six water mol­ecules as a hexaaqua cation. The occurrence of O—H...O and O—H...Cl hydrogen bonds results in a supra­molecular three-dimensional network.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.046
• wR factor = 0.084
• Data-to-parameter ratio = 18.3

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.95
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Zn2

Alert level G
ABSTM02_ALERT_3_G  When printed, the submitted absorption T values will be
            replaced by the scaled T values. Since the ratio of scaled T's
            is identical to the ratio of reported T values, the scaling
            does not imply a change to the absorption corrections used in
            the study.
            Ratio of Tmax expected/reported      0.946
            Tmax scaled      0.559 Tmin scaled      0.348
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           27.48
           From the CIF: _reflns_number_total               2748
           Count of symmetry unique reflns         1585
           Completeness (_total/calc)            173.38%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      1163
           Fraction of Friedel pairs measured     0.734
           Are heavy atom types Z>Si present        yes
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K

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

   2 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
   2 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97.

catena-Poly[bis[[dichlorozinc(II)]-µ-pyridine-4-carboxylato-κ²N,O] hexaaquazinc(II) dihydrate]

Crystal data

[ZnCl2(C6H4NO2)]2[Zn(H2O)6]·2H2O	F(000) = 2912
Mr = 726.24	Dx = 1.865 Mg m^−3
Orthorhombic, Fdd2	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: F 2 -2d	Cell parameters from 10770 reflections
a = 11.332 (7) Å	θ = 6.3–55.0°
b = 50.73 (2) Å	µ = 3.23 mm^−1
c = 9.001 (3) Å	T = 293 K
V = 5174 (4) Å^3	Block, colourless
Z = 8	0.39 × 0.19 × 0.18 mm

Data collection

Rigaku R-AXIS RAPID diffractometer	2748 independent reflections
Radiation source: fine-focus sealed tube	2402 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.075
ω scans	θmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −14→14
Tmin = 0.368, Tmax = 0.591	k = −65→61
12107 measured reflections	l = −11→10

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)] = 0.046	H-atom parameters constrained
wR(F^2) = 0.084	w = 1/[σ^2(Fo^2) + (0.0001P)^2 + 10.5079P] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max = 0.001
2748 reflections	Δρmax = 0.70 e Å^−3
150 parameters	Δρmin = −0.63 e Å^−3
4 restraints	Absolute structure: Flack (1983), with 1163 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.004 (17)

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
C1	0.3355 (5)	0.15480 (8)	0.3543 (5)	0.0344 (10)
H1	0.3481	0.1726	0.3362	0.041*
C2	0.3747 (5)	0.13661 (8)	0.2508 (4)	0.0325 (11)
H2	0.4129	0.1422	0.1650	0.039*
C3	0.3567 (5)	0.11016 (9)	0.2761 (4)	0.0296 (10)
C4	0.3944 (5)	0.08943 (9)	0.1660 (5)	0.0326 (10)
C5	0.2994 (5)	0.10270 (8)	0.4059 (5)	0.0348 (11)
H5	0.2859	0.0850	0.4266	0.042*
C6	0.2627 (5)	0.12213 (9)	0.5039 (5)	0.0352 (11)
H6	0.2242	0.1171	0.5907	0.042*
Cl1	0.03988 (15)	0.18695 (3)	0.51484 (14)	0.0499 (4)
Cl2	0.34190 (15)	0.20682 (2)	0.65898 (14)	0.0481 (3)
N	0.2805 (4)	0.14768 (7)	0.4787 (4)	0.0305 (8)
O1	0.3854 (4)	0.06616 (6)	0.1993 (4)	0.0506 (11)
O2	0.4296 (4)	0.09813 (7)	0.0418 (4)	0.0429 (10)
O3	0.1713 (5)	0.21220 (8)	0.2134 (4)	0.0647 (14)
H31	0.1185	0.2086	0.2769	0.097*
H32	0.1584	0.2034	0.1337	0.097*
O4	0.3675 (4)	0.24046 (10)	0.3724 (5)	0.0707 (13)
H41	0.4398	0.2385	0.3490	0.106*
H42	0.3551	0.2315	0.4507	0.106*
O5	0.3576 (5)	0.23517 (8)	0.0471 (5)	0.0681 (15)
H51	0.3615	0.2188	0.0407	0.102*
H52	0.3505	0.2426	−0.0355	0.102*
O6	0.5993 (4)	0.23227 (7)	0.3175 (4)	0.0495 (10)
H62	0.6208	0.2405	0.2395	0.074*
H61	0.6357	0.2171	0.3264	0.074*
Zn1	0.21056 (6)	0.174718 (10)	0.62187 (5)	0.03463 (15)
Zn2	0.2500	0.2500	0.21057 (8)	0.0382 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.046 (3)	0.027 (2)	0.031 (2)	−0.0008 (19)	0.004 (2)	−0.0005 (17)
C2	0.038 (3)	0.036 (2)	0.023 (2)	−0.001 (2)	0.0049 (18)	0.0022 (17)
C3	0.032 (3)	0.033 (2)	0.024 (2)	−0.0002 (19)	−0.0032 (18)	−0.0029 (16)
C4	0.034 (3)	0.035 (2)	0.029 (2)	−0.001 (2)	0.0007 (17)	−0.0040 (17)
C5	0.047 (3)	0.027 (2)	0.031 (2)	0.001 (2)	0.008 (2)	0.0013 (16)
C6	0.046 (3)	0.033 (2)	0.027 (2)	0.003 (2)	0.0106 (19)	0.0012 (16)
Cl1	0.0520 (10)	0.0503 (7)	0.0474 (7)	0.0145 (6)	0.0011 (6)	0.0010 (5)
Cl2	0.0585 (11)	0.0428 (6)	0.0431 (7)	−0.0101 (6)	0.0044 (6)	0.0007 (5)
N	0.037 (3)	0.0306 (18)	0.0243 (17)	−0.0002 (16)	0.0026 (15)	−0.0031 (14)
O1	0.080 (4)	0.0298 (17)	0.0424 (19)	0.0003 (17)	0.018 (2)	−0.0026 (14)
O2	0.062 (3)	0.0408 (19)	0.0255 (15)	0.0020 (17)	0.0161 (15)	−0.0006 (13)
O3	0.090 (4)	0.051 (2)	0.052 (2)	−0.029 (2)	0.024 (2)	−0.0099 (17)
O4	0.044 (3)	0.103 (3)	0.066 (3)	0.001 (2)	−0.004 (2)	0.044 (3)
O5	0.084 (4)	0.057 (2)	0.063 (2)	0.032 (2)	0.034 (3)	0.0191 (19)
O6	0.055 (3)	0.045 (2)	0.048 (2)	0.0055 (19)	0.0027 (18)	−0.0047 (15)
Zn1	0.0503 (4)	0.0286 (2)	0.0250 (2)	0.0023 (2)	0.0098 (2)	−0.00005 (19)
Zn2	0.0366 (5)	0.0387 (4)	0.0394 (4)	0.0002 (4)	0.000	0.000

Geometric parameters (Å, º)

C1—N	1.331 (6)	O2—Zn1^i	1.951 (3)
C1—C2	1.384 (6)	O3—Zn2	2.115 (4)
C1—H1	0.9300	O3—H31	0.8469
C2—C3	1.377 (6)	O3—H32	0.8564
C2—H2	0.9300	O4—Zn2	2.032 (4)
C3—C5	1.389 (6)	O4—H41	0.8516
C3—C4	1.507 (6)	O4—H42	0.8495
C4—O1	1.222 (6)	O5—Zn2	2.053 (4)
C4—O2	1.266 (5)	O5—H51	0.8356
C5—C6	1.387 (6)	O5—H52	0.8365
C5—H5	0.9300	O6—H62	0.8521
C6—N	1.331 (6)	O6—H61	0.8777
C6—H6	0.9300	Zn1—O2^ii	1.951 (3)
Cl1—Zn1	2.2481 (19)	Zn2—O4^iii	2.032 (4)
Cl2—Zn1	2.2315 (17)	Zn2—O5^iii	2.053 (4)
N—Zn1	2.043 (4)	Zn2—O3^iii	2.115 (4)
N—C1—C2	122.4 (4)	H41—O4—H42	107.6
N—C1—H1	118.8	Zn2—O5—H51	116.5
C2—C1—H1	118.8	Zn2—O5—H52	114.5
C3—C2—C1	119.4 (4)	H51—O5—H52	113.0
C3—C2—H2	120.3	H62—O6—H61	111.8
C1—C2—H2	120.3	O2^ii—Zn1—N	99.53 (15)
C2—C3—C5	118.3 (4)	O2^ii—Zn1—Cl2	115.87 (13)
C2—C3—C4	121.9 (4)	N—Zn1—Cl2	109.01 (13)
C5—C3—C4	119.7 (4)	O2^ii—Zn1—Cl1	110.19 (14)
O1—C4—O2	125.4 (4)	N—Zn1—Cl1	104.41 (12)
O1—C4—C3	119.3 (4)	Cl2—Zn1—Cl1	115.89 (7)
O2—C4—C3	115.3 (4)	O4—Zn2—O4^iii	88.4 (3)
C6—C5—C3	118.8 (4)	O4—Zn2—O5	92.2 (2)
C6—C5—H5	120.6	O4^iii—Zn2—O5	171.83 (19)
C3—C5—H5	120.6	O4—Zn2—O5^iii	171.83 (19)
N—C6—C5	122.5 (4)	O4^iii—Zn2—O5^iii	92.2 (2)
N—C6—H6	118.7	O5—Zn2—O5^iii	88.5 (3)
C5—C6—H6	118.7	O4—Zn2—O3^iii	86.03 (18)
C6—N—C1	118.6 (4)	O4^iii—Zn2—O3^iii	92.97 (19)
C6—N—Zn1	119.1 (3)	O5—Zn2—O3^iii	95.2 (2)
C1—N—Zn1	122.0 (3)	O5^iii—Zn2—O3^iii	85.80 (18)
C4—O2—Zn1^i	122.8 (3)	O4—Zn2—O3	92.97 (19)
Zn2—O3—H31	120.0	O4^iii—Zn2—O3	86.03 (18)
Zn2—O3—H32	122.2	O5—Zn2—O3	85.80 (18)
H31—O3—H32	109.5	O5^iii—Zn2—O3	95.2 (2)
Zn2—O4—H41	118.7	O3^iii—Zn2—O3	178.6 (2)
Zn2—O4—H42	127.8

Symmetry codes: (i) x+1/4, −y+1/4, z−3/4; (ii) x−1/4, −y+1/4, z+3/4; (iii) −x+1/2, −y+1/2, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H31···Cl1	0.85	2.57	3.349 (4)	154
O3—H32···O1^iv	0.86	1.95	2.808 (5)	178
O4—H41···O6	0.85	1.86	2.705 (7)	174
O4—H42···Cl2	0.85	2.26	3.106 (4)	174
O5—H51···Cl1^v	0.84	2.60	3.215 (4)	132
O5—H52···O6^vi	0.84	1.93	2.691 (5)	152
O6—H61···Cl2^v	0.88	2.83	3.356 (5)	120
O6—H61···O1^vii	0.88	2.02	2.759 (5)	142

Symmetry codes: (iv) x−1/4, −y+1/4, z−1/4; (v) x+1/2, y, z−1/2; (vi) −x+1, −y+1/2, z−1/2; (vii) x+1/4, −y+1/4, z+1/4.