A two-dimensional brick-wall layer barium(II) coordination polymer: poly[[tetra­aqua­barium(II)-di-μ-1H-imidazole-4,5-dicarboxyl­ato] dihydrate]

Gao, S.; Huo, L.-H.; Zhang, X.-F.; Zhao, H.

doi:10.1107/S1600536805035464

A two-dimensional brick-wall layer barium(II) coordination polymer: poly[[tetraaquabarium(II)-di-μ-1H-imidazole-4,5-dicarboxylato] dihydrate]

X.-F. Zhang, S. Gao, L.-H. Huo and H. Zhao

In the title two-dimensional coordination polymer, {[Ba(H₂IDC)₂(H₂O)₄]·2H₂O}_n (H₂IDC⁻ is the 1H-imidazole-4,5-dicarboxylate monoanion, C₅H₃N₂O₄⁻), each Ba^II atom, which lies on a crystallographic twofold rotation axis, is ten-coordinated by four O atoms and two N atoms from different H₂IDC⁻ ligands, as well as four water molecules, thus defining a hexadecahedron. Four Ba^II atoms are linked by four different H₂IDC⁻ ligands to produce a centrosymmetric macrocyclic structure, leading to an extended two-dimensional brick-wall open framework. Furthermore, there are π–π stacking interactions between adjacent parallel imidazole rings in the layer structure, and a three-dimensional supramolecular network is constructed via hydrogen-bonding and π–π stacking interactions.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805035464/cf6471sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536805035464/cf6471Isup2.hkl Contains datablock I

CCDC reference: 293851

checkCIF report

Key indicators

Single-crystal X-ray study
T = 295 K
Mean (C-C) = 0.002 Å
R factor = 0.016
wR factor = 0.037
Data-to-parameter ratio = 13.5

checkCIF/PLATON results

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Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          6

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

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

Computing details top

Data collection: RAPID-AUTO (Rigaku Corporation, 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: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

poly[[tetraaquabarium(II)-di-µ-1H-imidazole-4,5-dicarboxylato] dihydrate] top

Crystal data top

[Ba(C₅H₃N₂O₄)₂(H₂O)₄]·2H₂O	F(000) = 1096
M_r = 555.61	D_x = 2.048 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -c 2yc	Cell parameters from 7944 reflections
a = 17.962 (4) Å	θ = 3.2–27.5°
b = 6.7649 (14) Å	µ = 2.29 mm⁻¹
c = 14.892 (3) Å	T = 295 K
β = 95.22 (3)°	Prism, colorless
V = 1802.0 (7) Å³	0.35 × 0.24 × 0.18 mm
Z = 4

Data collection top

Rigaku R-AXIS RAPID diffractometer	2069 independent reflections
Radiation source: fine-focus sealed tube	1947 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.018
Detector resolution: 10 pixels mm^-1	θ_max = 27.5°, θ_min = 3.2°
ω scans	h = −23→23
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −8→8
T_min = 0.521, T_max = 0.665	l = −18→19
8564 measured reflections

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)] = 0.016	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.037	H atoms treated by a mixture of independent and constrained refinement
S = 1.10	w = 1/[σ²(F_o²) + (0.0169P)² + 2.0363P] where P = (F_o² + 2F_c²)/3
2069 reflections	(Δ/σ)_max = 0.001
153 parameters	Δρ_max = 0.33 e Å⁻³
10 restraints	Δρ_min = −0.46 e Å⁻³

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
Ba1	0.5000	0.509100 (19)	0.2500	0.01840 (5)
O1	0.09076 (7)	0.6583 (2)	0.24979 (9)	0.0298 (3)
O2	0.15823 (7)	0.6199 (2)	0.38126 (8)	0.0307 (3)
O3	0.29051 (7)	0.5978 (3)	0.44071 (8)	0.0341 (3)
H3	0.2440 (6)	0.608 (4)	0.4245 (17)	0.051*
O4	0.39967 (7)	0.5698 (2)	0.38621 (9)	0.0319 (3)
O1W	0.54233 (8)	0.3565 (2)	0.43014 (9)	0.0343 (3)
H1W1	0.5780 (10)	0.280 (3)	0.4191 (15)	0.051*
H1W2	0.5534 (13)	0.412 (4)	0.4807 (11)	0.051*
O2W	0.48618 (8)	0.8602 (2)	0.14398 (10)	0.0345 (3)
H2W1	0.5271 (9)	0.894 (4)	0.1248 (17)	0.052*
H2W2	0.4697 (13)	0.951 (3)	0.1752 (16)	0.052*
O3W	0.09162 (9)	0.6186 (3)	0.03906 (10)	0.0502 (4)
H3W1	0.0886 (17)	0.597 (5)	−0.0170 (8)	0.075*
H3W2	0.0600 (14)	0.706 (4)	0.0507 (18)	0.075*
N1	0.33901 (8)	0.6019 (2)	0.20987 (10)	0.0247 (3)
N2	0.21985 (8)	0.6213 (2)	0.15798 (9)	0.0242 (3)
H2	0.1808	0.6281	0.1202	0.029*
C1	0.29111 (10)	0.6111 (3)	0.13752 (12)	0.0279 (4)
H1	0.3050	0.6106	0.0789	0.033*
C2	0.22079 (9)	0.6187 (2)	0.24976 (11)	0.0195 (3)
C3	0.29519 (9)	0.6059 (2)	0.28118 (10)	0.0190 (3)
C4	0.15125 (9)	0.6331 (2)	0.29562 (12)	0.0231 (3)
C5	0.33180 (9)	0.5905 (3)	0.37362 (11)	0.0224 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ba1	0.01388 (7)	0.02323 (8)	0.01796 (7)	0.000	0.00079 (4)	0.000
O1	0.0168 (6)	0.0372 (7)	0.0347 (7)	0.0030 (5)	−0.0011 (5)	−0.0047 (6)
O2	0.0205 (6)	0.0464 (8)	0.0259 (6)	0.0039 (6)	0.0060 (5)	0.0005 (6)
O3	0.0213 (6)	0.0626 (9)	0.0186 (6)	0.0081 (6)	0.0029 (5)	0.0025 (6)
O4	0.0176 (6)	0.0544 (8)	0.0232 (6)	0.0055 (6)	−0.0005 (5)	−0.0018 (6)
O1W	0.0287 (7)	0.0475 (8)	0.0259 (7)	0.0128 (6)	−0.0018 (5)	−0.0058 (6)
O2W	0.0367 (8)	0.0336 (7)	0.0342 (7)	0.0036 (6)	0.0088 (6)	0.0003 (6)
O3W	0.0434 (9)	0.0720 (12)	0.0323 (8)	0.0143 (8)	−0.0128 (7)	−0.0170 (8)
N1	0.0207 (7)	0.0341 (8)	0.0197 (7)	0.0034 (6)	0.0036 (5)	0.0000 (6)
N2	0.0222 (7)	0.0315 (8)	0.0181 (7)	0.0040 (6)	−0.0033 (5)	−0.0016 (6)
C1	0.0270 (9)	0.0383 (10)	0.0185 (8)	0.0039 (8)	0.0031 (7)	−0.0011 (8)
C2	0.0196 (8)	0.0195 (7)	0.0193 (7)	0.0017 (6)	0.0007 (6)	−0.0008 (6)
C3	0.0175 (8)	0.0216 (7)	0.0179 (7)	0.0016 (6)	0.0022 (6)	−0.0001 (6)
C4	0.0176 (8)	0.0224 (8)	0.0293 (9)	0.0006 (6)	0.0018 (6)	−0.0030 (7)
C5	0.0196 (8)	0.0271 (8)	0.0204 (8)	0.0031 (6)	0.0016 (6)	−0.0011 (7)

Geometric parameters (Å, º) top

Ba1—N1	2.9662 (16)	C2—C4	1.481 (2)
Ba1—N1ⁱ	2.9662 (16)	C3—C5	1.474 (2)
Ba1—O1ⁱⁱ	2.8793 (14)	N1—C1	1.318 (2)
Ba1—O1ⁱⁱⁱ	2.8793 (14)	N1—C3	1.379 (2)
Ba1—O1W	2.9104 (15)	N2—C1	1.344 (2)
Ba1—O1Wⁱ	2.9104 (15)	N2—C2	1.366 (2)
Ba1—O2W	2.8501 (15)	N2—H2	0.860
Ba1—O2Wⁱ	2.8501 (15)	O1—Ba1^iv	2.8793 (14)
Ba1—O4	2.8629 (15)	O1W—H1W1	0.85 (2)
Ba1—O4ⁱ	2.8629 (15)	O1W—H1W2	0.85 (3)
O1—C4	1.241 (2)	O2W—H2W1	0.84 (3)
O2—C4	1.273 (2)	O2W—H2W2	0.84 (2)
O3—C5	1.298 (2)	O3—H3	0.85 (2)
O4—C5	1.224 (2)	O3W—H3W1	0.85 (2)
C1—H1	0.930	O3W—H3W2	0.85 (3)
C2—C3	1.378 (2)

O1ⁱⁱ—Ba1—N1	135.72 (4)	O2Wⁱ—Ba1—O4	61.10 (4)
O1ⁱⁱ—Ba1—N1ⁱ	68.47 (4)	O4ⁱ—Ba1—N1	119.46 (4)
O1ⁱⁱ—Ba1—O1ⁱⁱⁱ	68.98 (5)	O4ⁱ—Ba1—N1ⁱ	56.46 (4)
O1ⁱⁱ—Ba1—O1W	66.93 (4)	O4ⁱ—Ba1—O1ⁱⁱⁱ	120.79 (4)
O1ⁱⁱ—Ba1—O1Wⁱ	78.87 (4)	O4ⁱ—Ba1—O1ⁱⁱ	74.00 (4)
O1W—Ba1—N1	115.40 (5)	O4ⁱ—Ba1—O1W	125.14 (4)
O1W—Ba1—N1ⁱ	73.82 (5)	O4ⁱ—Ba1—O1Wⁱ	61.72 (4)
O1Wⁱ—Ba1—O1W	138.44 (6)	Ba1—O1W—H1W1	100.2 (16)
O2W—Ba1—N1	71.21 (5)	Ba1—O1W—H1W2	133.1 (19)
O2W—Ba1—N1ⁱ	88.24 (5)	Ba1—O2W—H2W1	112.2 (18)
O2W—Ba1—O1ⁱⁱⁱ	131.81 (4)	Ba1—O2W—H2W2	108.7 (18)
O2W—Ba1—O1ⁱⁱ	134.99 (4)	O1—C4—C2	119.24 (16)
O2W—Ba1—O1W	143.96 (4)	O1—C4—O2	124.19 (16)
O2W—Ba1—O1Wⁱ	77.45 (4)	O2—C4—C2	116.56 (15)
O2Wⁱ—Ba1—O2W	67.13 (6)	O3—C5—C3	118.58 (15)
O2W—Ba1—O4	104.15 (4)	O4—C5—C3	120.29 (15)
O4—Ba1—N1ⁱ	119.46 (4)	O4—C5—O3	121.13 (16)
O4—Ba1—N1	56.46 (4)	N1—C1—H1	123.8
O4—Ba1—O1ⁱⁱ	120.79 (4)	N1—C1—N2	112.42 (15)
O4—Ba1—O1ⁱⁱⁱ	74.00 (4)	N1—C3—C5	118.72 (14)
O4—Ba1—O1Wⁱ	125.14 (4)	N2—C1—H1	123.8
O4—Ba1—O1W	61.72 (4)	N2—C2—C3	105.31 (14)
O4ⁱ—Ba1—O4	163.52 (7)	N2—C2—C4	121.79 (15)
N1ⁱ—Ba1—N1	155.55 (6)	C1—N1—Ba1	136.61 (11)
O1ⁱⁱⁱ—Ba1—N1ⁱ	135.72 (4)	C1—N1—C3	104.65 (14)
O1ⁱⁱⁱ—Ba1—N1	68.47 (4)	C1—N2—C2	107.51 (14)
O1ⁱⁱⁱ—Ba1—O1Wⁱ	66.93 (4)	C1—N2—H2	126.2
O1ⁱⁱⁱ—Ba1—O1W	78.87 (4)	C2—C3—C5	131.15 (15)
O1Wⁱ—Ba1—N1ⁱ	115.40 (5)	C2—C3—N1	110.10 (15)
O1Wⁱ—Ba1—N1	73.82 (5)	C2—N2—H2	126.2
O2Wⁱ—Ba1—N1ⁱ	71.21 (5)	C3—C2—C4	132.87 (15)
O2Wⁱ—Ba1—N1	88.24 (5)	C3—N1—Ba1	117.61 (11)
O2Wⁱ—Ba1—O1ⁱⁱ	131.81 (4)	C4—O1—Ba1^iv	125.45 (11)
O2Wⁱ—Ba1—O1ⁱⁱⁱ	134.99 (4)	C5—O3—H3	113.6 (17)
O2Wⁱ—Ba1—O1Wⁱ	143.96 (4)	C5—O4—Ba1	126.16 (11)
O2Wⁱ—Ba1—O1W	77.45 (4)	H1W1—O1W—H1W2	108.7 (15)
O2Wⁱ—Ba1—O4ⁱ	104.15 (4)	H2W1—O2W—H2W2	110.5 (15)
O2W—Ba1—O4ⁱ	61.10 (4)	H3W1—O3W—H3W2	109.8 (16)

Ba1—N1—C1—N2	167.07 (12)	N2—C2—C3—N1	0.36 (19)
Ba1—N1—C3—C2	−170.21 (10)	N2—C2—C4—O1	−3.7 (2)
Ba1—N1—C3—C5	8.0 (2)	N2—C2—C4—O2	176.78 (16)
Ba1^iv—O1—C4—C2	−112.59 (15)	O1ⁱⁱ—Ba1—N1—C1	−71.19 (19)
Ba1^iv—O1—C4—O2	66.9 (2)	O1ⁱⁱⁱ—Ba1—N1—C1	−88.10 (19)
Ba1—O4—C5—C3	−6.3 (2)	O1ⁱⁱⁱ—Ba1—N1—C3	77.55 (12)
Ba1—O4—C5—O3	173.15 (13)	O1ⁱⁱ—Ba1—N1—C3	94.46 (13)
C1—N1—C3—C2	−0.3 (2)	O1ⁱⁱ—Ba1—O4—C5	−120.12 (15)
C1—N1—C3—C5	177.85 (16)	O1ⁱⁱⁱ—Ba1—O4—C5	−67.36 (16)
C1—N2—C2—C3	−0.23 (18)	O1W—Ba1—N1—C1	−153.46 (18)
C1—N2—C2—C4	178.41 (16)	O1Wⁱ—Ba1—N1—C1	−17.02 (18)
C2—C3—C5—O3	−3.5 (3)	O1W—Ba1—N1—C3	12.19 (14)
C2—C3—C5—O4	176.00 (18)	O1Wⁱ—Ba1—N1—C3	148.63 (13)
C2—N2—C1—N1	0.0 (2)	O1W—Ba1—O4—C5	−153.13 (17)
C3—C2—C4—O1	174.48 (18)	O1Wⁱ—Ba1—O4—C5	−21.81 (18)
C3—C2—C4—O2	−5.0 (3)	O2Wⁱ—Ba1—N1—C1	131.33 (19)
C3—N1—C1—N2	0.2 (2)	O2W—Ba1—N1—C1	64.92 (18)
C4—C2—C3—C5	4.0 (3)	O2W—Ba1—N1—C3	−129.43 (13)
C4—C2—C3—N1	−178.07 (17)	O2Wⁱ—Ba1—N1—C3	−63.02 (12)
N1ⁱ—Ba1—N1—C1	99.14 (18)	O2Wⁱ—Ba1—O4—C5	116.00 (17)
N1ⁱ—Ba1—N1—C3	−95.21 (12)	O2W—Ba1—O4—C5	62.65 (16)
N1ⁱ—Ba1—O4—C5	158.74 (15)	O4—Ba1—N1—C1	−172.7 (2)
N1—Ba1—O4—C5	7.10 (15)	O4ⁱ—Ba1—N1—C1	26.0 (2)
N1—C3—C5—O3	178.80 (17)	O4ⁱ—Ba1—N1—C3	−168.30 (11)
N1—C3—C5—O4	−1.7 (3)	O4—Ba1—N1—C3	−7.06 (11)
N2—C2—C3—C5	−177.53 (17)	O4ⁱ—Ba1—O4—C5	87.85 (16)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3···O2	0.85 (2)	1.62 (2)	2.4635 (19)	173 (3)
N2—H2···O3W	0.86	1.92	2.775 (2)	175
O1W—H1W1···O2ⁱⁱ	0.85 (2)	1.93 (2)	2.7752 (19)	174 (2)
O1W—H1W2···O4^v	0.85 (3)	2.09 (3)	2.880 (2)	156 (2)
O2W—H2W1···O3W^vi	0.84 (3)	2.36 (3)	3.102 (3)	148 (2)
O2W—H2W2···O1^vii	0.84 (2)	2.15 (2)	2.980 (2)	170 (2)
O3W—H3W2···O1W^vii	0.85 (3)	2.14 (2)	2.965 (2)	163 (3)
O3W—H3W1···O2W^viii	0.85 (2)	2.24 (2)	2.951 (2)	142 (2)
O3W—H3W1···O2^ix	0.84 (2)	2.52 (2)	3.173 (2)	135 (2)

Symmetry codes: (ii) x+1/2, y−1/2, z; (v) −x+1, −y+1, −z+1; (vi) x+1/2, y+1/2, z; (vii) −x+1/2, y+1/2, −z+1/2; (viii) −x+1/2, −y+3/2, −z; (ix) x, −y+1, z−1/2.

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A two-dimensional brick-wall layer barium(II) coordination polymer: poly[[tetra­aqua­barium(II)-di-μ-1H-imidazole-4,5-dicarboxyl­ato] dihydrate]

Supporting information

Key indicators

checkCIF/PLATON results

A two-dimensional brick-wall layer barium(II) coordination polymer: poly[[tetraaquabarium(II)-di-μ-1H-imidazole-4,5-dicarboxylato] dihydrate]