Literature DB >> 22199627

Poly[(aqua-calcium)-μ(4)-pyrazine-2,3-di-carboxyl-ato].

Qing-Feng Yang, Yue-Ping Zhang, Jing Lu, Ping Xue, Zheng Wang.

Abstract

The polymeric title compound, [Ca(C(6)H(2)N(2)O(4))(H(2)O)](n), was synthesized from pyrazine-2,3-dicarb-oxy-lic acid and calcium dichloride under hydro-thermal conditions. The Ca(2+) cation is seven-coordinated by five O atoms and one N atom of four pyrazine-2,3-dicarboxyl-ate anions, and one water mol-ecule. The complete deprotonated pyrazine-2,3-dicarboxyl-ate anion adopts a μ(4)-coordination mode, resulting in the formation of a three-dimensional structure.

Entities: Chemical Disease Species

Year: 2011 PMID： 22199627 PMCID： PMC3238750 DOI： 10.1107/S1600536811050276

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

For transition and lanthanide metal complexes containing the pydc ligand (pydc = pyrazine-2,3-dicarboxylate), see: Chen et al. (2008 ▶); Hu et al. (2004 ▶); Kitaura et al. (2002 ▶); Ma et al. (2006 ▶); Sakagami-Yoshida et al. (2000 ▶); Yin (2009 ▶); Zou et al. (1999 ▶).

Experimental

Crystal data

[Ca(C6H2N2O4)(H2O)] M = 224.19 Monoclinic, a = 6.8109 (7) Å b = 12.0469 (13) Å c = 9.9191 (11) Å β = 102.333 (1)° V = 795.08 (15) Å3 Z = 4 Mo Kα radiation μ = 0.79 mm−1 T = 298 K 0.35 × 0.25 × 0.10 mm

Data collection

Bruker SMART APEX CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2005) ▶ T min = 0.770, T max = 0.926 3904 measured reflections 1405 independent reflections 1210 reflections with I > 2σ(I) R int = 0.026

Refinement

R[F 2 > 2σ(F 2)] = 0.028 wR(F 2) = 0.075 S = 1.06 1405 reflections 143 parameters All H-atom parameters refined Δρmax = 0.35 e Å−3 Δρmin = −0.34 e Å−3 Data collection: SMART (Bruker, 2005 ▶); cell refinement: SAINT (Bruker, 2005 ▶); data reduction: SAINT; 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: SHELXL97 ▶. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811050276/ds2152sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811050276/ds2152Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Ca(C₆H₂N₂O₄)(H₂O)]	F(000) = 456
M_r = 224.19	D_x = 1.873 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 2583 reflections
a = 6.8109 (7) Å	θ = 2.7–28.2°
b = 12.0469 (13) Å	µ = 0.79 mm⁻¹
c = 9.9191 (11) Å	T = 298 K
β = 102.333 (1)°	Block, colorless
V = 795.08 (15) Å³	0.35 × 0.25 × 0.10 mm
Z = 4

Bruker SMART APEX CCD diffractometer	1405 independent reflections
Radiation source: fine-focus sealed tube	1210 reflections with I > 2σ(I)
graphite	R_int = 0.026
ω scans	θ_max = 25.0°, θ_min = 2.7°
Absorption correction: multi-scan (SADABS; Bruker, 2005)	h = −8→8
T_min = 0.770, T_max = 0.926	k = −12→14
3904 measured reflections	l = −10→11

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)] = 0.028	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.075	All H-atom parameters refined
S = 1.06	w = 1/[σ²(F_o²) + (0.0386P)² + 0.4192P] where P = (F_o² + 2F_c²)/3
1405 reflections	(Δ/σ)_max < 0.001
143 parameters	Δρ_max = 0.35 e Å⁻³
0 restraints	Δρ_min = −0.34 e Å⁻³

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.

	x	y	z	U_iso*/U_eq
O5	0.2040 (3)	−0.20134 (16)	0.40189 (19)	0.0390 (5)
O2	0.2816 (2)	0.22697 (11)	0.83932 (14)	0.0279 (4)
O4	0.4176 (2)	0.09317 (12)	0.37610 (18)	0.0343 (4)
N2	0.2587 (3)	0.37894 (14)	0.64192 (17)	0.0218 (4)
C4	0.2491 (4)	0.45523 (18)	0.5424 (2)	0.0268 (5)
Ca1	0.23561 (6)	−0.08343 (3)	0.59754 (4)	0.01641 (15)
O3	0.1145 (2)	0.06496 (11)	0.41707 (14)	0.0207 (3)
O1	0.3116 (2)	0.08934 (10)	0.69619 (14)	0.0256 (4)
C6	0.2677 (3)	0.12378 (16)	0.41813 (19)	0.0170 (4)
C1	0.2679 (3)	0.27200 (15)	0.60607 (19)	0.0173 (4)
C5	0.2868 (3)	0.18869 (15)	0.72322 (19)	0.0181 (4)
C2	0.2662 (3)	0.24255 (16)	0.46930 (19)	0.0171 (4)
N1	0.2632 (3)	0.31989 (14)	0.37173 (17)	0.0238 (4)
C3	0.2526 (4)	0.42579 (17)	0.4091 (2)	0.0284 (5)
H2	0.242 (3)	0.526 (2)	0.564 (2)	0.024 (6)*
H1	0.245 (3)	0.479 (2)	0.336 (2)	0.029 (6)*
H3	0.212 (5)	−0.198 (3)	0.319 (4)	0.072 (11)*
H4	0.207 (5)	−0.260 (3)	0.426 (4)	0.073 (12)*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
O5	0.0702 (13)	0.0292 (10)	0.0187 (9)	−0.0027 (9)	0.0122 (8)	−0.0006 (7)
O2	0.0484 (10)	0.0199 (8)	0.0161 (7)	0.0005 (7)	0.0082 (7)	−0.0016 (6)
O4	0.0211 (9)	0.0356 (9)	0.0487 (10)	−0.0014 (7)	0.0130 (7)	−0.0179 (7)
N2	0.0281 (10)	0.0171 (8)	0.0193 (9)	0.0012 (7)	0.0034 (7)	−0.0005 (7)
C4	0.0397 (14)	0.0160 (10)	0.0243 (11)	0.0017 (9)	0.0062 (10)	0.0023 (9)
Ca1	0.0167 (2)	0.0162 (2)	0.0158 (2)	−0.00003 (14)	0.00219 (16)	−0.00004 (14)
O3	0.0178 (7)	0.0215 (7)	0.0225 (7)	−0.0037 (6)	0.0035 (6)	−0.0001 (6)
O1	0.0408 (9)	0.0156 (7)	0.0190 (8)	0.0019 (6)	0.0031 (7)	−0.0007 (5)
C6	0.0179 (11)	0.0208 (10)	0.0110 (9)	0.0009 (8)	0.0002 (8)	0.0008 (8)
C1	0.0176 (10)	0.0175 (10)	0.0164 (10)	0.0002 (8)	0.0028 (8)	−0.0012 (8)
C5	0.0192 (10)	0.0171 (10)	0.0170 (10)	−0.0008 (8)	0.0016 (8)	−0.0019 (8)
C2	0.0144 (10)	0.0202 (10)	0.0162 (10)	−0.0013 (8)	0.0023 (8)	0.0003 (8)
N1	0.0292 (10)	0.0233 (9)	0.0184 (8)	−0.0005 (7)	0.0043 (7)	0.0016 (7)
C3	0.0422 (14)	0.0208 (11)	0.0215 (12)	−0.0003 (9)	0.0055 (10)	0.0059 (9)

O5—Ca1	2.3774 (17)	Ca1—O2^iv	2.3779 (14)
O5—H3	0.83 (4)	Ca1—O3	2.5396 (14)
O5—H4	0.74 (4)	Ca1—N2^iv	2.6159 (17)
O2—C5	1.248 (2)	Ca1—Ca1ⁱⁱⁱ	3.9284 (8)
O2—Ca1ⁱ	2.3779 (14)	Ca1—H4	2.70 (4)
O4—C6	1.238 (2)	O3—C6	1.260 (2)
O4—Ca1ⁱⁱ	2.3233 (15)	O3—Ca1ⁱⁱⁱ	2.3682 (14)
N2—C4	1.340 (3)	O1—C5	1.246 (2)
N2—C1	1.341 (3)	C6—C2	1.519 (3)
N2—Ca1ⁱ	2.6159 (17)	C1—C2	1.400 (3)
C4—C3	1.374 (3)	C1—C5	1.520 (3)
C4—H2	0.88 (2)	C2—N1	1.340 (2)
Ca1—O1	2.3111 (14)	N1—C3	1.335 (3)
Ca1—O4ⁱⁱ	2.3233 (15)	C3—H1	0.96 (2)
Ca1—O3ⁱⁱⁱ	2.3682 (14)

Ca1—O5—H3	139 (2)	O3ⁱⁱⁱ—Ca1—Ca1ⁱⁱⁱ	38.35 (3)
Ca1—O5—H4	108 (3)	O5—Ca1—Ca1ⁱⁱⁱ	88.95 (5)
H3—O5—H4	112 (3)	O2^iv—Ca1—Ca1ⁱⁱⁱ	122.70 (4)
C5—O2—Ca1ⁱ	127.64 (12)	O3—Ca1—Ca1ⁱⁱⁱ	35.36 (3)
C6—O4—Ca1ⁱⁱ	150.28 (14)	N2^iv—Ca1—Ca1ⁱⁱⁱ	114.42 (4)
C4—N2—C1	117.46 (18)	O1—Ca1—H4	162.6 (8)
C4—N2—Ca1ⁱ	126.65 (14)	O4ⁱⁱ—Ca1—H4	88.1 (7)
C1—N2—Ca1ⁱ	115.89 (12)	O3ⁱⁱⁱ—Ca1—H4	95.7 (7)
N2—C4—C3	121.6 (2)	O5—Ca1—H4	15.2 (8)
N2—C4—H2	118.6 (14)	O2^iv—Ca1—H4	53.8 (8)
C3—C4—H2	119.8 (14)	O3—Ca1—H4	98.1 (8)
O1—Ca1—O4ⁱⁱ	82.39 (5)	N2^iv—Ca1—H4	117.9 (8)
O1—Ca1—O3ⁱⁱⁱ	94.17 (5)	Ca1ⁱⁱⁱ—Ca1—H4	98.7 (8)
O4ⁱⁱ—Ca1—O3ⁱⁱⁱ	176.20 (5)	C6—O3—Ca1ⁱⁱⁱ	140.29 (13)
O1—Ca1—O5	148.96 (6)	C6—O3—Ca1	104.26 (11)
O4ⁱⁱ—Ca1—O5	88.53 (7)	Ca1ⁱⁱⁱ—O3—Ca1	106.29 (5)
O3ⁱⁱⁱ—Ca1—O5	95.26 (6)	C5—O1—Ca1	158.12 (14)
O1—Ca1—O2^iv	140.60 (5)	O4—C6—O3	124.80 (18)
O4ⁱⁱ—Ca1—O2^iv	91.60 (6)	O4—C6—C2	117.25 (17)
O3ⁱⁱⁱ—Ca1—O2^iv	90.05 (5)	O3—C6—C2	117.90 (16)
O5—Ca1—O2^iv	68.91 (6)	N2—C1—C2	120.60 (17)
O1—Ca1—O3	70.98 (5)	N2—C1—C5	115.63 (16)
O4ⁱⁱ—Ca1—O3	106.51 (5)	C2—C1—C5	123.74 (17)
O3ⁱⁱⁱ—Ca1—O3	73.71 (5)	O1—C5—O2	125.83 (18)
O5—Ca1—O3	83.45 (6)	O1—C5—C1	117.58 (17)
O2^iv—Ca1—O3	146.61 (5)	O2—C5—C1	116.55 (16)
O1—Ca1—N2^iv	77.47 (5)	N1—C2—C1	121.28 (18)
O4ⁱⁱ—Ca1—N2^iv	94.59 (6)	N1—C2—C6	114.43 (16)
O3ⁱⁱⁱ—Ca1—N2^iv	83.05 (5)	C1—C2—C6	124.29 (17)
O5—Ca1—N2^iv	133.04 (6)	C3—N1—C2	117.23 (17)
O2^iv—Ca1—N2^iv	64.18 (5)	N1—C3—C4	121.8 (2)
O3—Ca1—N2^iv	138.80 (5)	N1—C3—H1	115.3 (14)
O1—Ca1—Ca1ⁱⁱⁱ	80.40 (4)	C4—C3—H1	122.9 (14)
O4ⁱⁱ—Ca1—Ca1ⁱⁱⁱ	141.75 (5)

4 in total

1. Polymeric aqua(nitrato-kappa(2)O,O')(1,10-phenanthroline-kappa(2)N,N')(2,3-pyrazinedicarboxylato-kappa(2)N,O)europium(III) monohydrate.

Authors: Mao Lin Hu; Ji Xin Yuan; Fan Chen; Qian Shi
Journal: Acta Crystallogr C Date: 2004-03-31 Impact factor: 1.172

2. A short history of SHELX.

Authors: George M Sheldrick
Journal: Acta Crystallogr A Date: 2007-12-21 Impact factor: 2.290

3. Anomalous stereochemistry of pyrazolato-3,5-dicarboxylato-bridged dinuclear chromate(III) complexes containing ethylenediamine-N,N'-dicarboxylates with entrapped unstable conformations: X-ray structure of Na[Cr2(eddp)(mu-pzdc)].6H2O.

Authors: N Sakagami-Yoshida; M Teramoto; A Hioki; A Fuyuhiro; S Kaizaki
Journal: Inorg Chem Date: 2000-12-11 Impact factor: 5.165

4. A new polymorph of catena-poly[[tri-aqua-cadmium(II)]-μ(2)-pyrazine-2,3-dicarboxyl-ato].

Authors: Hua Yin
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2009-07-22

4 in total