catena-Poly[[[triaqua­(4,5-diaza­fluorene-9-one)cadmium]-μ-benzene-1,3-dicarboxyl­ato] dihydrate]

Li, X.-P.; Fang, W.; Mei, Z.-M.; Jin, X.-J.; Qi, W.-L.

doi:10.1107/S1600536809031237

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 65| Part 9| September 2009| Pages m1069-m1070

doi:10.1107/S1600536809031237

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catena-Poly[[[triaqua(4,5-diazafluorene-9-one)cadmium]-μ-benzene-1,3-dicarboxylato] dihydrate]

Xiao-Ping Li,^a Wei Fang,^a ^* Ze-Min Mei,^a Xiang-Jun Jin ^a and Wen-Liang Qi ^b

^aDepartment of Chemistry, Baicheng Normal University, Baicheng 137000, People's Republic of China, and ^bSiping Academy of Science and Technology, Siping 136000, People's Republic of China
^*Correspondence e-mail: fangwei1026@yahoo.com.cn

(Received 9 July 2009; accepted 7 August 2009; online 15 August 2009)

In the title compound, {[Cd(C₈H₄O₄)(C₁₁H₆N₂O)(H₂O)₃]·2H₂O}_n, the Cd^II atom is seven-coordinated by two N atoms from the phenanthroline-derived 4,5-diazafluorene-9-one ligand, two O atoms from one bidentate benzene-1,3-dicarboxylate ligand and three O atoms from the three water molecules in a distorted pentagonal-bipyramidal arrangement. Moreover, there are two dissociative water molecules in each unit. Neighbouring units interact through π–π interactions [centroid–centroid distances = 3.325 (3) and 3.358 (4) Å] and O—H⋯O hydrogen-bonding, resulting in a two-dimensional network extending parallel to (001).

Related literature

The 1,10-phenanthroline (phen) ligand has been widely used to build novel supramolecular architectures through its aromatic π–π interations, see: Chen & Liu (2002 ). The phen derivative 4,5-diazafluorene-9-one was recently shown to form a coordination polymer with a distinctive supramolecular architecture, see: Kraft et al. (2002 ). For the ligand synthesis, see: Henderson et al. (1984 ).

Experimental

Crystal data

[Cd(C₈H₄O₄)(C₁₁H₆N₂O)(H₂O)₃]·2H₂O
M_r = 548.78
Triclinic, $[P \overline 1]$
a = 6.9383 (10) Å
b = 10.8070 (16) Å
c = 14.429 (2) Å
α = 96.268 (2)°
β = 92.602 (2)°
γ = 102.019 (2)°
V = 1049.3 (3) Å³
Z = 2
Mo Kα radiation
μ = 1.10 mm⁻¹
T = 293 K
0.34 × 0.29 × 0.20 mm

Data collection

Bruker APEXII diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 1998 ) T_min = 0.697, T_max = 0.804
5319 measured reflections
3804 independent reflections
3260 reflections with I > 2σ(I)
R_int = 0.017

Refinement

R[F² > 2σ(F²)] = 0.037
wR(F²) = 0.093
S = 1.05
3804 reflections
284 parameters
H-atom parameters constrained
Δρ_max = 1.39 e Å⁻³
Δρ_min = −0.64 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

Cd1—O7	2.271 (3)
Cd1—O6	2.326 (3)
Cd1—O2	2.354 (3)
Cd1—O5	2.368 (3)
Cd1—O1	2.441 (3)
Cd1—N2	2.472 (3)
Cd1—N1	2.492 (3)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—HO5A⋯O3ⁱ	0.85	1.95	2.728 (4)	151
O5—HO5B⋯O4ⁱⁱ	0.96	2.06	2.933 (4)	151
O6—HO6A⋯OW1ⁱⁱⁱ	0.92	1.86	2.776 (5)	175
O6—HO6B⋯O4ⁱⁱ	0.99	1.70	2.675 (4)	171
O7—HO7A⋯O4^iv	0.91	1.96	2.744 (4)	143
O7—HO7B⋯OW2	0.91	1.87	2.757 (4)	162
OW1—HW1A⋯O8^v	0.89	2.07	2.903 (5)	156
OW1—HW1B⋯O1^vi	0.90	2.12	2.824 (5)	135
OW2—HW2A⋯O3^vii	0.99	1.80	2.769 (4)	168
OW2—HW2B⋯O2^viii	0.95	1.99	2.936 (5)	173
Symmetry codes: (i) -x, -y+1, -z; (ii) x, y+1, z; (iii) -x, -y+1, -z+1; (iv) x+1, y+1, z; (v) -x+1, -y+2, -z+1; (vi) -x+1, -y+1, -z+1; (vii) -x+1, -y+1, -z; (viii) x+1, y, z.

Data collection: APEX2 (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXL97; software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809031237/jh2092sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809031237/jh2092Isup2.hkl

checkCIF report

Comment top

The 1,10-phenanthroline (phen) ligand has been widely used to build novel supramolecular architectures through its aromatic π-π interations (Chen & Liu, 2002). The phen derivative 4,5-diazafluorene-9-one (C₁₁H₆N₂O; L), was recently shown to form a coordination polymer with a distinctive supramolecular architecture (Kraft et al., 2002). We selected benzene-1,3-dicarboxylate (C₈H₄O₄^2-; 1,3-BDC) to act as a metal-metal linker in its deprotonated form and L as a secondary ligand, generating the title compound, [Cd(C₁₁H₆N₂O)(C₈H₄O₄)(H₂O)₃.2H₂O], a new coordinationg polymer, which is reported here. In compound (I), the Cd^II atom of unit is surrounded by two N atoms derived from the bidentate L ligand, two O atom from a bidentate 1,3-BDC ligand and three O atoms from three H₂O moleculars. This results in a very distorted CdN₂O₅ pentagonal bipyramid with the donor atoms of both the bidentate species occupying both an equatorial and an axial site (Table 1, Fig.1). The average Cd—O and Cd—N distances are 2.352 (3) and 2.482 (3) Å, respectively. Neighbouring units in (I) are connectede through π-π interactions between L ligands with π-π stacking distances of 3.325 (3) and 3.358 (4) Å, resulting in a two-dimensional supramolecular structure. Finally, interunit OW—H···O hydrogen bonds (Table 2) complete the structure of (I).

Related literature top

The 1,10-phenanthroline (phen) ligand has been widely used to build novel supramolecular architectures through its aromatic π–π interations, see: Chen & Liu (2002). The phen derivative 4,5-diazafluorene-9-one was recently shown to form a coordination polymer with a distinctive supramolecular architecture, see: Kraft et al. (2002). For the ligand synthesis, see: Henderson et al. (1984).

Experimental top

Ligand L was synthesized according to the literature method. (Henderson et al., 1984). A mixture of CdCl₂ (0.3 mmol), L(0.1 mmol) and H₂1,3-BDC (0.3 mmol) in distilled water (30 ml) was stirred thoroughly for 1 h at ambient temperature. The pH was adjusted to 7.5 with aqueous NaOH solution. The suspension was then sealed in a Teflon-lined stainless steel reaction vessel (40 ml). The reaction was performed under autogeneous pressure and static conditions in an oven at 443 K for 4.5 d. The vessel was then cooled slowly inside the oven to 298 K at a rate of 5 K h^-1 before opening: yellow crystals of (I) were collected.

Computing details top

Data collection: APEX2 (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXL97 (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. view of the local coordination of Cd(II) with the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. (arbitrary spheres for the H atoms).
	Fig. 2. A view of the two-dimensional supramolecular structure of (I) generated by π-π interactions.

catena-Poly[[[triaqua(4,5-diazafluorene-9-one)cadmium]-µ- benzene-1,3-dicarboxylato] dihydrate] top

Crystal data top

[Cd(C₈H₄O₄)(C₁₁H₆N₂O)(H₂O)₃]·2H₂O	Z = 2
M_r = 548.78	F(000) = 552.0
Triclinic, P1	D_x = 1.737 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.9383 (10) Å	Cell parameters from 25 reflections
b = 10.8070 (16) Å	θ = 7.5–15°
c = 14.429 (2) Å	µ = 1.10 mm⁻¹
α = 96.268 (2)°	T = 293 K
β = 92.602 (2)°	Block, yellow
γ = 102.019 (2)°	0.34 × 0.29 × 0.20 mm
V = 1049.3 (3) Å³

Data collection top

Bruker APEXII diffractometer	3804 independent reflections
Radiation source: fine-focus sealed tube	3260 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.017
Detector resolution: 0 pixels mm^-1	θ_max = 25.3°, θ_min = 1.4°
ω scans	h = −8→6
Absorption correction: multi-scan (SADABS; Bruker, 1998)	k = −12→12
T_min = 0.697, T_max = 0.804	l = −17→15
5319 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)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.093	H-atom parameters constrained
S = 1.05	w = 1/[σ²(F_o²) + (0.0466P)² + 0.937P] where P = (F_o² + 2F_c²)/3
3804 reflections	(Δ/σ)_max < 0.001
284 parameters	Δρ_max = 1.39 e Å⁻³
0 restraints	Δρ_min = −0.64 e Å⁻³

Crystal data top

[Cd(C₈H₄O₄)(C₁₁H₆N₂O)(H₂O)₃]·2H₂O	γ = 102.019 (2)°
M_r = 548.78	V = 1049.3 (3) Å³
Triclinic, P1	Z = 2
a = 6.9383 (10) Å	Mo Kα radiation
b = 10.8070 (16) Å	µ = 1.10 mm⁻¹
c = 14.429 (2) Å	T = 293 K
α = 96.268 (2)°	0.34 × 0.29 × 0.20 mm
β = 92.602 (2)°

Data collection top

Bruker APEXII diffractometer	3804 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 1998)	3260 reflections with I > 2σ(I)
T_min = 0.697, T_max = 0.804	R_int = 0.017
5319 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	0 restraints
wR(F²) = 0.093	H-atom parameters constrained
S = 1.05	Δρ_max = 1.39 e Å⁻³
3804 reflections	Δρ_min = −0.64 e Å⁻³
284 parameters

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
Cd1	0.41915 (4)	0.92090 (2)	0.19901 (2)	0.03260 (12)
O1	0.4624 (5)	0.7585 (3)	0.2984 (2)	0.0506 (8)
O2	0.2646 (5)	0.7034 (3)	0.1714 (2)	0.0507 (8)
O3	0.0030 (5)	0.2413 (3)	0.0709 (2)	0.0466 (7)
O4	0.0050 (4)	0.1021 (2)	0.1719 (2)	0.0448 (7)
O5	0.2170 (4)	0.9328 (3)	0.06495 (19)	0.0423 (7)
HO5A	0.1523	0.8617	0.0376	0.051*
HO5B	0.1310	0.9904	0.0785	0.051*
O6	0.1543 (4)	0.9578 (3)	0.28319 (19)	0.0409 (7)
HO6A	0.0652	0.8878	0.2978	0.049*
HO6B	0.0857	1.0067	0.2439	0.049*
O7	0.6983 (4)	0.8944 (3)	0.1303 (2)	0.0423 (7)
HO7A	0.7909	0.9616	0.1164	0.051*
HO7B	0.7246	0.8150	0.1185	0.051*
O8	0.8494 (5)	1.5000 (3)	0.3739 (3)	0.0547 (8)
OW1	0.1330 (6)	0.2440 (4)	0.6739 (3)	0.0680 (10)*
HW1A	0.1594	0.3283	0.6755	0.082*
HW1B	0.2287	0.1998	0.6674	0.082*
OW2	0.8579 (5)	0.6822 (3)	0.0952 (2)	0.0534 (8)
HW2A	0.9077	0.6971	0.0335	0.064*
HW2B	0.9856	0.6831	0.1226	0.064*
N1	0.6184 (5)	1.0507 (3)	0.3377 (2)	0.0365 (8)
N2	0.5214 (5)	1.1420 (3)	0.1616 (2)	0.0328 (7)
C1	0.6800 (7)	1.0281 (4)	0.4218 (3)	0.0478 (11)
H1A	0.6541	0.9443	0.4352	0.057*
C2	0.7803 (8)	1.1222 (5)	0.4906 (3)	0.0562 (13)
H2A	0.8212	1.1006	0.5478	0.067*
C3	0.8193 (7)	1.2488 (5)	0.4736 (3)	0.0482 (11)
H3A	0.8847	1.3138	0.5188	0.058*
C4	0.7579 (6)	1.2732 (4)	0.3883 (3)	0.0341 (9)
C5	0.7763 (6)	1.3928 (4)	0.3402 (3)	0.0389 (10)
C6	0.6842 (6)	1.3482 (4)	0.2420 (3)	0.0354 (9)
C7	0.6627 (6)	1.4071 (4)	0.1647 (3)	0.0451 (11)
H7A	0.7073	1.4946	0.1656	0.054*
C8	0.5715 (7)	1.3310 (5)	0.0844 (3)	0.0487 (11)
H8	0.5559	1.3670	0.0296	0.058*
C9	0.5033 (6)	1.2005 (4)	0.0861 (3)	0.0404 (10)
H9A	0.4419	1.1517	0.0316	0.049*
C10	0.6136 (5)	1.2180 (3)	0.2354 (3)	0.0291 (8)
C11	0.6594 (6)	1.1723 (4)	0.3241 (3)	0.0320 (8)
C12	0.3421 (6)	0.6768 (4)	0.2441 (3)	0.0362 (9)
C13	0.2920 (5)	0.5422 (4)	0.2679 (3)	0.0318 (8)
C14	0.3450 (6)	0.5166 (4)	0.3568 (3)	0.0362 (9)
H14A	0.4113	0.5820	0.4014	0.043*
C15	0.2974 (6)	0.3917 (4)	0.3781 (3)	0.0411 (10)
H15A	0.3312	0.3737	0.4375	0.049*
C16	0.2012 (6)	0.2952 (4)	0.3122 (3)	0.0338 (9)
H16A	0.1704	0.2121	0.3273	0.041*
C17	0.1493 (5)	0.3197 (3)	0.2233 (3)	0.0276 (8)
C18	0.1937 (5)	0.4439 (3)	0.2020 (3)	0.0309 (8)
H19A	0.1573	0.4615	0.1428	0.037*
C19	0.0452 (5)	0.2137 (3)	0.1493 (3)	0.0311 (8)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.03412 (18)	0.02318 (16)	0.03710 (18)	0.00121 (11)	−0.00345 (12)	0.00067 (11)
O1	0.0498 (19)	0.0243 (15)	0.069 (2)	−0.0032 (13)	−0.0120 (16)	−0.0015 (14)
O2	0.055 (2)	0.0298 (16)	0.063 (2)	0.0004 (14)	−0.0124 (16)	0.0103 (14)
O3	0.0568 (19)	0.0375 (16)	0.0360 (17)	−0.0061 (14)	−0.0068 (14)	−0.0016 (13)
O4	0.0468 (18)	0.0216 (14)	0.061 (2)	0.0021 (12)	−0.0168 (15)	0.0021 (13)
O5	0.0478 (18)	0.0318 (15)	0.0423 (17)	0.0043 (13)	−0.0111 (13)	−0.0030 (12)
O6	0.0420 (16)	0.0411 (16)	0.0401 (16)	0.0089 (13)	0.0007 (13)	0.0081 (13)
O7	0.0371 (16)	0.0300 (15)	0.0556 (18)	0.0009 (12)	0.0049 (14)	−0.0019 (13)
O8	0.0515 (19)	0.0296 (17)	0.076 (2)	0.0010 (14)	−0.0073 (17)	−0.0039 (15)
OW2	0.0510 (19)	0.0481 (19)	0.061 (2)	0.0056 (15)	0.0053 (16)	0.0144 (16)
N1	0.0396 (19)	0.0273 (17)	0.0382 (19)	−0.0008 (14)	0.0019 (15)	0.0008 (14)
N2	0.0299 (17)	0.0321 (18)	0.0330 (18)	0.0024 (14)	−0.0027 (14)	−0.0014 (14)
C1	0.067 (3)	0.038 (2)	0.039 (2)	0.009 (2)	0.002 (2)	0.011 (2)
C2	0.069 (3)	0.060 (3)	0.036 (3)	0.009 (3)	−0.006 (2)	0.010 (2)
C3	0.049 (3)	0.051 (3)	0.038 (2)	0.002 (2)	−0.005 (2)	−0.007 (2)
C4	0.027 (2)	0.034 (2)	0.036 (2)	0.0024 (16)	0.0011 (16)	−0.0111 (17)
C5	0.028 (2)	0.029 (2)	0.055 (3)	0.0015 (17)	0.0003 (18)	−0.0055 (19)
C6	0.027 (2)	0.0250 (19)	0.053 (3)	0.0035 (16)	0.0016 (18)	0.0025 (18)
C7	0.039 (2)	0.031 (2)	0.065 (3)	0.0043 (19)	0.002 (2)	0.013 (2)
C8	0.040 (2)	0.062 (3)	0.050 (3)	0.018 (2)	0.004 (2)	0.020 (2)
C9	0.039 (2)	0.044 (2)	0.036 (2)	0.0053 (19)	0.0006 (18)	0.0020 (19)
C10	0.0218 (18)	0.0279 (19)	0.036 (2)	0.0036 (15)	0.0032 (15)	−0.0014 (16)
C11	0.030 (2)	0.027 (2)	0.036 (2)	0.0012 (16)	0.0006 (16)	−0.0024 (16)
C12	0.030 (2)	0.025 (2)	0.051 (3)	0.0025 (17)	0.0037 (19)	0.0002 (18)
C13	0.0259 (19)	0.027 (2)	0.041 (2)	0.0049 (16)	0.0000 (16)	0.0001 (16)
C14	0.039 (2)	0.030 (2)	0.037 (2)	0.0061 (17)	−0.0036 (18)	−0.0050 (17)
C15	0.045 (2)	0.045 (2)	0.034 (2)	0.011 (2)	−0.0019 (18)	0.0073 (19)
C16	0.035 (2)	0.0262 (19)	0.042 (2)	0.0084 (17)	0.0033 (17)	0.0063 (17)
C17	0.0238 (18)	0.0235 (18)	0.035 (2)	0.0036 (15)	0.0008 (15)	0.0021 (15)
C18	0.028 (2)	0.0264 (19)	0.036 (2)	0.0041 (16)	0.0003 (16)	0.0010 (16)
C19	0.0247 (19)	0.024 (2)	0.043 (2)	0.0039 (15)	0.0011 (17)	−0.0023 (17)

Geometric parameters (Å, º) top

Cd1—O7	2.271 (3)	C1—H1A	0.9300
Cd1—O6	2.326 (3)	C2—C3	1.388 (7)
Cd1—O2	2.354 (3)	C2—H2A	0.9300
Cd1—O5	2.368 (3)	C3—C4	1.356 (6)
Cd1—O1	2.441 (3)	C3—H3A	0.9300
Cd1—N2	2.472 (3)	C4—C11	1.388 (5)
Cd1—N1	2.492 (3)	C4—C5	1.517 (6)
Cd1—C12	2.736 (4)	C5—C6	1.514 (6)
O1—C12	1.254 (5)	C6—C7	1.361 (6)
O2—C12	1.246 (5)	C6—C10	1.381 (5)
O3—C19	1.238 (5)	C7—C8	1.388 (7)
O4—C19	1.262 (5)	C7—H7A	0.9300
O5—HO5A	0.8494	C8—C9	1.394 (6)
O5—HO5B	0.9593	C8—H8	0.9300
O6—HO6A	0.9221	C9—H9A	0.9300
O6—HO6B	0.9864	C10—C11	1.466 (6)
O7—HO7A	0.9108	C12—C13	1.505 (5)
O7—HO7B	0.9138	C13—C18	1.384 (5)
O8—C5	1.203 (5)	C13—C14	1.390 (6)
OW1—HW1A	0.8890	C14—C15	1.393 (6)
OW1—HW1B	0.8979	C14—H14A	0.9300
OW2—HW2A	0.9870	C15—C16	1.369 (6)
OW2—HW2B	0.9517	C15—H15A	0.9300
N1—C11	1.324 (5)	C16—C17	1.385 (5)
N1—C1	1.333 (5)	C16—H16A	0.9300
N2—C10	1.321 (5)	C17—C18	1.385 (5)
N2—C9	1.332 (5)	C17—C19	1.514 (5)
C1—C2	1.388 (7)	C18—H19A	0.9300

O7—Cd1—O6	174.04 (10)	C4—C3—H3A	121.5
O7—Cd1—O2	94.34 (11)	C2—C3—H3A	121.5
O6—Cd1—O2	89.02 (11)	C3—C4—C11	118.9 (4)
O7—Cd1—O5	99.74 (11)	C3—C4—C5	134.3 (4)
O6—Cd1—O5	85.55 (10)	C11—C4—C5	106.8 (4)
O2—Cd1—O5	82.74 (10)	O8—C5—C6	127.8 (4)
O7—Cd1—O1	88.67 (11)	O8—C5—C4	126.7 (4)
O6—Cd1—O1	89.30 (11)	C6—C5—C4	105.5 (3)
O2—Cd1—O1	54.28 (10)	C7—C6—C10	118.1 (4)
O5—Cd1—O1	136.81 (10)	C7—C6—C5	134.3 (4)
O7—Cd1—N2	83.60 (10)	C10—C6—C5	107.6 (3)
O6—Cd1—N2	95.28 (10)	C6—C7—C8	117.1 (4)
O2—Cd1—N2	156.30 (11)	C6—C7—H7A	121.4
O5—Cd1—N2	74.40 (10)	C8—C7—H7A	121.4
O1—Cd1—N2	148.78 (10)	C7—C8—C9	119.9 (4)
O7—Cd1—N1	90.91 (11)	C7—C8—H8	120.1
O6—Cd1—N1	83.18 (11)	C9—C8—H8	120.1
O2—Cd1—N1	131.53 (11)	N2—C9—C8	123.6 (4)
O5—Cd1—N1	143.43 (10)	N2—C9—H9A	118.2
O1—Cd1—N1	77.78 (10)	C8—C9—H9A	118.2
N2—Cd1—N1	72.17 (11)	N2—C10—C6	127.1 (4)
O7—Cd1—C12	92.22 (11)	N2—C10—C11	123.2 (3)
O6—Cd1—C12	88.55 (11)	C6—C10—C11	109.7 (3)
O2—Cd1—C12	27.01 (11)	N1—C11—C4	126.0 (4)
O5—Cd1—C12	109.62 (11)	N1—C11—C10	123.7 (3)
O1—Cd1—C12	27.27 (11)	C4—C11—C10	110.3 (3)
N2—Cd1—C12	174.70 (11)	O2—C12—O1	122.2 (4)
N1—Cd1—C12	104.75 (12)	O2—C12—C13	119.4 (4)
C12—O1—Cd1	89.6 (3)	O1—C12—C13	118.4 (4)
C12—O2—Cd1	93.9 (2)	O2—C12—Cd1	59.1 (2)
Cd1—O5—HO5A	115.3	O1—C12—Cd1	63.1 (2)
Cd1—O5—HO5B	111.3	C13—C12—Cd1	177.9 (3)
HO5A—O5—HO5B	110.7	C18—C13—C14	119.9 (4)
Cd1—O6—HO6A	117.7	C18—C13—C12	120.4 (4)
Cd1—O6—HO6B	104.4	C14—C13—C12	119.6 (4)
HO6A—O6—HO6B	109.4	C13—C14—C15	119.1 (4)
Cd1—O7—HO7A	122.1	C13—C14—H14A	120.4
Cd1—O7—HO7B	120.4	C15—C14—H14A	120.4
HO7A—O7—HO7B	117.4	C16—C15—C14	120.5 (4)
HW1A—OW1—HW1B	121.2	C16—C15—H15A	119.8
HW2A—OW2—HW2B	93.1	C14—C15—H15A	119.8
C11—N1—C1	114.5 (4)	C15—C16—C17	120.7 (4)
C11—N1—Cd1	109.7 (3)	C15—C16—H16A	119.6
C1—N1—Cd1	135.7 (3)	C17—C16—H16A	119.6
C10—N2—C9	114.2 (3)	C16—C17—C18	119.1 (3)
C10—N2—Cd1	110.7 (2)	C16—C17—C19	121.4 (3)
C9—N2—Cd1	135.1 (3)	C18—C17—C19	119.5 (3)
N1—C1—C2	124.0 (4)	C13—C18—C17	120.6 (4)
N1—C1—H1A	118.0	C13—C18—H19A	119.7
C2—C1—H1A	118.0	C17—C18—H19A	119.7
C1—C2—C3	119.7 (4)	O3—C19—O4	123.9 (4)
C1—C2—H2A	120.2	O3—C19—C17	118.5 (3)
C3—C2—H2A	120.2	O4—C19—C17	117.5 (3)
C4—C3—C2	117.0 (4)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—HO5A···O3ⁱ	0.85	1.95	2.728 (4)	151
O5—HO5B···O4ⁱⁱ	0.96	2.06	2.933 (4)	151
O6—HO6A···OW1ⁱⁱⁱ	0.92	1.86	2.776 (5)	175
O6—HO6B···O4ⁱⁱ	0.99	1.70	2.675 (4)	171
O7—HO7A···O4^iv	0.91	1.96	2.744 (4)	143
O7—HO7B···OW2	0.91	1.87	2.757 (4)	162
OW1—HW1A···O8^v	0.89	2.07	2.903 (5)	156
OW1—HW1B···O1^vi	0.90	2.12	2.824 (5)	135
OW2—HW2A···O3^vii	0.99	1.80	2.769 (4)	168
OW2—HW2B···O2^viii	0.95	1.99	2.936 (5)	173

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

Experimental details

Crystal data
Chemical formula	[Cd(C₈H₄O₄)(C₁₁H₆N₂O)(H₂O)₃]·2H₂O
M_r	548.78
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	6.9383 (10), 10.8070 (16), 14.429 (2)
α, β, γ (°)	96.268 (2), 92.602 (2), 102.019 (2)
V (Å³)	1049.3 (3)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.10
Crystal size (mm)	0.34 × 0.29 × 0.20

Data collection
Diffractometer	Bruker APEXII diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 1998)
T_min, T_max	0.697, 0.804
No. of measured, independent and observed [I > 2σ(I)] reflections	5319, 3804, 3260
R_int	0.017
(sin θ/λ)_max (Å⁻¹)	0.600

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.093, 1.05
No. of reflections	3804
No. of parameters	284
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.39, −0.64

Computer programs: APEX2 (Bruker, 1998), SAINT (Bruker, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top

Cd1—O7	2.271 (3)	Cd1—O1	2.441 (3)
Cd1—O6	2.326 (3)	Cd1—N2	2.472 (3)
Cd1—O2	2.354 (3)	Cd1—N1	2.492 (3)
Cd1—O5	2.368 (3)

O7—Cd1—O6	174.04 (10)	O7—Cd1—O1	88.67 (11)
O7—Cd1—O2	94.34 (11)	O6—Cd1—O1	89.30 (11)
O6—Cd1—O2	89.02 (11)	O2—Cd1—O1	54.28 (10)
O7—Cd1—O5	99.74 (11)	O5—Cd1—O1	136.81 (10)
O6—Cd1—O5	85.55 (10)	N2—Cd1—N1	72.17 (11)
O2—Cd1—O5	82.74 (10)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—HO5A···O3ⁱ	0.85	1.95	2.728 (4)	150.9
O5—HO5B···O4ⁱⁱ	0.96	2.06	2.933 (4)	151.1
O6—HO6A···OW1ⁱⁱⁱ	0.92	1.86	2.776 (5)	174.5
O6—HO6B···O4ⁱⁱ	0.99	1.70	2.675 (4)	170.7
O7—HO7A···O4^iv	0.91	1.96	2.744 (4)	143.2
O7—HO7B···OW2	0.91	1.87	2.757 (4)	162.3
OW1—HW1A···O8^v	0.89	2.07	2.903 (5)	155.6
OW1—HW1B···O1^vi	0.90	2.12	2.824 (5)	134.6
OW2—HW2A···O3^vii	0.99	1.80	2.769 (4)	167.9
OW2—HW2B···O2^viii	0.95	1.99	2.936 (5)	172.9

Acknowledgements

The authors thank Baicheng Normal University for supporting this work.

References

Bruker (1998). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Chen, X.-M. & Liu, G.-F. (2002). Chem. Eur. J. 8, 4811–4817. CrossRef PubMed CAS Google Scholar
Henderson, L. J., Fronczek, F. R. & Cherry, W. R. (1984). J. Am. Chem. Soc. 106, 5876–5879. CSD CrossRef CAS Web of Science Google Scholar
Kraft, B. J., Eppley, H. J., Huffman, J. C. & Zaleski, J. M. (2002). J. Am. Chem. Soc. 124, 272–280. Web of Science CSD CrossRef PubMed CAS Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar

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Volume 65| Part 9| September 2009| Pages m1069-m1070

doi:10.1107/S1600536809031237

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

catena-Poly[[[tri­aqua­(4,5-di­aza­fluorene-9-one)cadmium]-μ-benzene-1,3-di­carboxyl­ato] dihydrate]

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Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

catena-Poly[[[triaqua(4,5-diazafluorene-9-one)cadmium]-μ-benzene-1,3-dicarboxylato] dihydrate]