Poly[[diaqua[μ4-4,4′-carbonylbis(benzene-1,2-dicarboxylato)]bis(dipyrido[3,2-a:2′,3′-c]phenazine)dicadmium(II)] monohydrate] (2024)

Issue contents

Download PDF of article

Download CIF

3D view

Navigation

1. Related literature
2. Experimental
Supporting Information
References

Highlighting
Dictionary of Crystallography
IUPAC Gold Book
more ...

Download citation

Article statistics

Issue contents

Download PDF of article

Download CIF

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 64| Part 6| June 2008| Pagesm810-m811

doi:10.1107/S1600536808013676

Openaccess

Poly[[diaqua[μ₄-4,4′-carbonylbis(benzene-1,2-dicarboxylato)]bis(dipyrido[3,2-a:2′,3′-c]phenazine)dicadmium(II)] monohydrate]

Xiao-Huan Yuan,a* Wen-Zhi Zhangb and Yan-Hui Chua

^aKey Laboratory for Anti-fibrosis Biotherapy of Heilongjiang, Mudanjiang Medical University, Mudanjiang 157011, Heilongjiang Province, People's Republic of China, and ^bCollege of Chemistry and Chemical Engineering, Qiqihar University, Qiqihar 161006, Heilongjiang Province, People's Republic of China
^*Correspondence e-mail: yuanxiaohuan1@yahoo.com.cn

(Received 19 April 2008; accepted 8 May 2008; online 14 May 2008)

In the title compound, {[Cd₂(C₁₇H₆O₉)(C₁₈H₁₀N₄)₂(H₂O)₂]·H₂O}_n, the Cd^II atom is seven-coordinated by five O atoms from two different 4,4′-carbonylbis(benzene-1,2-dicarboxylate) (BPTC) anions and one water molecule, and by two N atoms from one chelating dipyrido[3,2-a:2′,3′-c]phenazine (L) ligand in a distorted pentagonal-bipyramidal geometry. The BPTC anions link the Cd^II atoms, forming a one-dimensional chain structure. The L ligands are attached on both sides of the chain. A twofold rotation axis passes through the complex molecule. The crystal structure involves O—H⋯O hydrogen bonds.

Related literature

For related literature, see: Li et al. (2007); Wu et al. (1997).

Experimental

Crystal data

[Cd₂(C₁₇H₆O₉)(C₁₈H₁₀N₄)₂(H₂O)₂]·H₂O
M_r = 1197.67
Monoclinic, P 2/n
a = 15.698 (3) Å
b = 6.7028 (13) Å
c = 21.428 (4) Å
β = 102.45 (3)°
V = 2201.7 (8) Å³
Z = 2
Mo Kα radiation
μ = 1.05 mm⁻¹
T = 293 (2) K
0.27 × 0.24 × 0.21 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) T_min = 0.742, T_max = 0.801
20222 measured reflections
5022 independent reflections
3508 reflections with I > 2σ(I)
R_int = 0.093

Refinement

R[F² > 2σ(F²)] = 0.049
wR(F²) = 0.125
S = 1.04
5022 reflections
352 parameters
6 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.70 e Å⁻³
Δρ_min = −0.84 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

Cd1—N1	2.352 (4)
Cd1—N2	2.367 (4)
Cd1—O1	2.381 (4)
Cd1—O2	2.411 (3)
Cd1—O1W	2.323 (4)
Cd1—O3ⁱ	2.321 (4)
Cd1—O5ⁱ	2.572 (4)

O3ⁱ—Cd1—O1W	102.56 (15)
O3ⁱ—Cd1—N1	84.39 (13)
O1W—Cd1—N1	102.54 (15)
O3ⁱ—Cd1—N2	154.84 (14)
O1W—Cd1—N2	82.23 (16)
N1—Cd1—N2	70.49 (14)
O3ⁱ—Cd1—O1	88.62 (13)
O1W—Cd1—O1	153.69 (14)
N1—Cd1—O1	102.20 (14)
N2—Cd1—O1	97.78 (14)
O3ⁱ—Cd1—O2	119.58 (12)
O1W—Cd1—O2	99.59 (13)
N1—Cd1—O2	142.59 (13)
N2—Cd1—O2	83.19 (13)
O1—Cd1—O2	54.58 (12)
O3ⁱ—Cd1—O5ⁱ	53.13 (13)
O1W—Cd1—O5ⁱ	82.76 (15)
N1—Cd1—O5ⁱ	136.94 (13)
N2—Cd1—O5ⁱ	151.32 (14)
O1—Cd1—O5ⁱ	85.29 (13)
O2—Cd1—O5ⁱ	75.40 (12)
Symmetry code: (i) x, y-1, z.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—HW11⋯O2ⁱⁱ	0.84 (4)	1.92 (3)	2.731 (5)	163 (6)
O1W—HW12⋯O5ⁱⁱ	0.84 (4)	2.23 (4)	2.892 (6)	136 (5)
O2W—HW22⋯O1ⁱ	0.85 (2)	2.14 (8)	2.913 (5)	152 (15)
Symmetry codes: (i) x, y-1, z; (ii) -x+1, -y+1, -z.

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

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808013676/rz2212sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808013676/rz2212Isup2.hkl

checkCIF report

Comment top

Dipyrido[3,2-a:2',3'-c]phenazine (L) has been widely used to recognize the secondary structure of DNA in rutenium(II) complexes (Wu et al., 1997). Recently, the L ligand has received intense interest in the chemistry of coordination polymers (Li et al., 2007). In the present paper, we selected H₄BPTC = 3,3',4,4'-benzophenone tetracarboxylic acid as a bridging ligand and L as a chelating ligand, generating a new cadmium(II) coordination polymer, [Cd₂(L)₂(BPTC)(H₂O)₂]^.2H₂O.

Selected bond lengths and angles for the title compound are given in Table 1. Each Cd^II atom is seven-coordinated by five O atoms from two different BPTC anions and one water molecule, and two N atoms from one chelating L ligand in a distorted pentagonal bipyramidal coordination geometry (Fig. 1). The BPTC anions link the Cd^II atoms to form a one-dimensional chain structure (Fig. 2). The L ligands are attached on both sides of the chain. Intermolecular O—H···O H-bonds (Table 2) and the π–π interactions (between L ligands of neighboring chains, with the shortest atom-to-atom distance of 3.43(2) Å) stabilize the crystal structure.

Related literature top

For related literature, see: Li et al. (2007); Wu et al. (1997).

Experimental top

Dipyrido[3,2 - a:2',3'-c]-phenazine (0.5 mmol) and 3,3',4,4'-benzophenone tetracarboxylic acid (0.25 mmol) were mixed with an aqueous solution (12 ml) of cadmium chloride dihydrate (0.5 mmol) with stirring. The solution was heated in a 25 ml Teflon-lined reaction vessel at 390 K for 120 h and then cooled to room temperature over a period of 16 h. Colourless crystals of the title compound were collected.

Refinement top

All H atoms on C atoms were positioned geometrically (C—H = 0.93 Å) and refined as riding, with U_iso(H) = 1.2U_eq(C). The water H atoms were located in a difference Fourier map and refined with a distance restraint of O–H = 0.85 Å, and with U_iso(H) = 1.2U_eq(O).

Computing details top

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

Figures top

	Fig. 1. The structure of the title compound , showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. Symmetry codes: (i) x, y - 1, z; (ii) 0.5 - x, y, 0.5 - z.
	Fig. 2. View of the chain structure of the title compound.

Poly[[diaqua[µ₄-4,4'-carbonylbis(benzene-1,2- dicarboxylato)]bis(dipyrido[3,2-a:2',3'-c]phenazine)dicadmium(II)] monohydrate] top

Crystal data

top

[Cd₂(C₁₇H₆O₉)(C₁₈H₁₀N₄)₂(H₂O)₂]·H₂O	F(000) = 1196
M_r = 1197.67	D_x = 1.807 Mg m⁻³
Monoclinic, P2/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yac	Cell parameters from 13844 reflections
a = 15.698 (3) Å	θ = 3.0–27.5°
b = 6.7028 (13) Å	µ = 1.05 mm⁻¹
c = 21.428 (4) Å	T = 293 K
β = 102.45 (3)°	Block, colourless
V = 2201.7 (8) Å³	0.27 × 0.24 × 0.21 mm
Z = 2

Data collection

top

Rigaku R-AXIS RAPID diffractometer	5022 independent reflections
Radiation source: rotating anode	3508 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.093
Detector resolution: 10.0 pixels mm^-1	θ_max = 27.5°, θ_min = 3.0°
ω scans	h = −20→18
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −8→8
T_min = 0.742, T_max = 0.801	l = −27→27
20222 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)] = 0.049	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.125	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ²(F_o²) + (0.0614P)²] where P = (F_o² + 2F_c²)/3
5022 reflections	(Δ/σ)_max < 0.001
352 parameters	Δρ_max = 0.70 e Å⁻³
6 restraints	Δρ_min = −0.84 e Å⁻³

Crystal data

top

[Cd₂(C₁₇H₆O₉)(C₁₈H₁₀N₄)₂(H₂O)₂]·H₂O	V = 2201.7 (8) Å³
M_r = 1197.67	Z = 2
Monoclinic, P2/n	Mo Kα radiation
a = 15.698 (3) Å	µ = 1.05 mm⁻¹
b = 6.7028 (13) Å	T = 293 K
c = 21.428 (4) Å	0.27 × 0.24 × 0.21 mm
β = 102.45 (3)°

Data collection

top

Rigaku R-AXIS RAPID diffractometer	5022 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	3508 reflections with I > 2σ(I)
T_min = 0.742, T_max = 0.801	R_int = 0.093
20222 measured reflections

Refinement

top

R[F² > 2σ(F²)] = 0.049	6 restraints
wR(F²) = 0.125	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	Δρ_max = 0.70 e Å⁻³
5022 reflections	Δρ_min = −0.84 e Å⁻³
352 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	Occ. (<1)
C1	0.7768 (4)	0.0149 (8)	0.1740 (2)	0.0342 (12)
H1	0.7343	−0.0638	0.1861	0.041*
C2	0.8642 (3)	−0.0462 (8)	0.1917 (3)	0.0377 (13)
H2	0.8794	−0.1597	0.2166	0.045*
C3	0.9266 (4)	0.0645 (8)	0.1717 (3)	0.0367 (12)
H3	0.9848	0.0255	0.1819	0.044*
C4	0.9015 (3)	0.2375 (7)	0.1356 (2)	0.0286 (11)
C5	0.8145 (3)	0.2937 (7)	0.1223 (2)	0.0261 (10)
C6	0.9661 (3)	0.3643 (8)	0.1135 (2)	0.0319 (11)
C7	0.9401 (4)	0.5492 (8)	0.0840 (2)	0.0339 (12)
C8	0.8467 (4)	0.6054 (7)	0.0703 (2)	0.0316 (12)
C9	0.7859 (3)	0.4772 (7)	0.0878 (2)	0.0281 (11)
C10	0.6728 (4)	0.6892 (8)	0.0431 (3)	0.0423 (14)
H10	0.6134	0.7174	0.0328	0.051*
C11	0.8165 (4)	0.7825 (8)	0.0393 (3)	0.0398 (13)
H11	0.8559	0.8716	0.0279	0.048*
C12	0.7312 (4)	0.8258 (8)	0.0259 (3)	0.0502 (17)
H12	0.7112	0.9446	0.0055	0.060*
C13	1.0803 (4)	0.6155 (10)	0.0777 (3)	0.0455 (15)
C14	1.1439 (5)	0.7468 (10)	0.0625 (3)	0.0604 (19)
H14	1.1280	0.8737	0.0466	0.072*
C15	1.2290 (5)	0.6847 (13)	0.0715 (3)	0.068 (2)
H15	1.2708	0.7707	0.0618	0.082*
C16	1.2537 (4)	0.4954 (12)	0.0950 (3)	0.0566 (19)
H16	1.3116	0.4562	0.0998	0.068*
C17	1.1943 (4)	0.3640 (12)	0.1113 (3)	0.0550 (17)
H17	1.2119	0.2383	0.1275	0.066*
C18	1.1052 (4)	0.4256 (9)	0.1028 (3)	0.0395 (13)
C19	0.5216 (3)	0.5601 (7)	0.1603 (3)	0.0300 (11)
C20	0.4599 (3)	0.6828 (7)	0.1904 (2)	0.0250 (10)
C21	0.4935 (3)	1.0024 (7)	0.1355 (2)	0.0298 (11)
C22	0.4394 (3)	0.8792 (7)	0.1726 (2)	0.0228 (10)
C23	0.3716 (3)	0.9765 (7)	0.1933 (2)	0.0264 (10)
H23	0.3585	1.1084	0.1817	0.032*
C24	0.3230 (3)	0.8755 (7)	0.2318 (2)	0.0270 (11)
C25	0.3484 (3)	0.6844 (7)	0.2525 (2)	0.0320 (12)
H25	0.3201	0.6192	0.2805	0.038*
C26	0.4164 (3)	0.5886 (7)	0.2315 (2)	0.0311 (11)
H26	0.4324	0.4598	0.2454	0.037*
C27	0.2500	0.9870 (11)	0.2500	0.0338 (17)
N1	0.7518 (3)	0.1804 (6)	0.1405 (2)	0.0292 (9)
N2	0.6995 (3)	0.5206 (6)	0.0737 (2)	0.0333 (10)
N3	0.9946 (3)	0.6766 (7)	0.0669 (2)	0.0419 (11)
N4	1.0483 (3)	0.2994 (7)	0.1226 (2)	0.0385 (11)
O1	0.5763 (2)	0.4504 (5)	0.19432 (18)	0.0386 (9)
O2	0.5089 (2)	0.5605 (5)	0.09996 (17)	0.0338 (8)
O1W	0.5801 (3)	0.2021 (6)	−0.00419 (19)	0.0457 (10)
HW11	0.563 (4)	0.287 (6)	−0.033 (2)	0.055*
HW12	0.553 (3)	0.096 (5)	−0.016 (3)	0.055*
O3	0.5736 (2)	0.9818 (6)	0.1491 (2)	0.0443 (10)
O4	0.2500	1.1681 (8)	0.2500	0.0448 (15)
O2W	0.7500	−0.3982 (12)	0.2500	0.082 (2)
HW22	0.708 (7)	−0.479 (19)	0.240 (8)	0.099*	0.50
HW21	0.764 (14)	−0.40 (2)	0.2906 (11)	0.099*	0.50
O5	0.4540 (3)	1.1233 (6)	0.0948 (2)	0.0506 (11)
Cd1	0.60585 (2)	0.27952 (5)	0.103914 (18)	0.02753 (13)

Atomic displacement parameters (Å²)

top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.034 (3)	0.038 (3)	0.032 (3)	−0.002 (2)	0.010 (3)	0.007 (2)
C2	0.033 (3)	0.039 (3)	0.040 (3)	0.003 (2)	0.006 (3)	0.013 (2)
C3	0.029 (3)	0.043 (3)	0.035 (3)	0.001 (2)	0.001 (3)	0.005 (2)
C4	0.028 (3)	0.031 (3)	0.028 (2)	−0.001 (2)	0.008 (2)	−0.004 (2)
C5	0.025 (2)	0.030 (2)	0.026 (2)	0.000 (2)	0.011 (2)	0.002 (2)
C6	0.024 (3)	0.043 (3)	0.030 (3)	−0.009 (2)	0.009 (2)	0.000 (2)
C7	0.035 (3)	0.037 (3)	0.032 (3)	−0.012 (2)	0.013 (3)	−0.005 (2)
C8	0.036 (3)	0.031 (3)	0.031 (3)	−0.009 (2)	0.014 (3)	0.000 (2)
C9	0.030 (3)	0.025 (2)	0.031 (3)	−0.003 (2)	0.010 (2)	0.000 (2)
C10	0.036 (3)	0.038 (3)	0.058 (4)	0.010 (2)	0.020 (3)	0.011 (3)
C11	0.046 (3)	0.030 (3)	0.046 (3)	−0.003 (2)	0.016 (3)	0.005 (2)
C12	0.063 (4)	0.028 (3)	0.065 (4)	0.008 (3)	0.026 (4)	0.018 (3)
C13	0.034 (3)	0.066 (4)	0.036 (3)	−0.023 (3)	0.008 (3)	−0.008 (3)
C14	0.051 (4)	0.073 (5)	0.061 (4)	−0.024 (4)	0.021 (4)	0.009 (3)
C15	0.041 (4)	0.110 (6)	0.056 (4)	−0.039 (4)	0.018 (4)	−0.002 (4)
C16	0.023 (3)	0.108 (6)	0.042 (4)	−0.019 (3)	0.013 (3)	−0.011 (4)
C17	0.033 (3)	0.095 (5)	0.038 (3)	−0.007 (3)	0.008 (3)	−0.001 (3)
C18	0.024 (3)	0.065 (4)	0.030 (3)	−0.010 (3)	0.008 (2)	−0.003 (3)
C19	0.027 (3)	0.027 (2)	0.040 (3)	0.002 (2)	0.015 (3)	0.002 (2)
C20	0.015 (2)	0.032 (3)	0.029 (2)	−0.0024 (18)	0.005 (2)	0.001 (2)
C21	0.033 (3)	0.028 (3)	0.031 (3)	−0.005 (2)	0.013 (2)	−0.004 (2)
C22	0.014 (2)	0.029 (2)	0.025 (2)	−0.0026 (18)	0.004 (2)	0.0002 (19)
C23	0.023 (3)	0.028 (2)	0.030 (3)	−0.0025 (19)	0.009 (2)	0.002 (2)
C24	0.020 (2)	0.033 (3)	0.031 (3)	−0.004 (2)	0.013 (2)	−0.002 (2)
C25	0.032 (3)	0.033 (3)	0.035 (3)	−0.005 (2)	0.015 (2)	0.004 (2)
C26	0.027 (3)	0.030 (2)	0.036 (3)	0.002 (2)	0.007 (2)	0.005 (2)
C27	0.036 (4)	0.038 (4)	0.030 (4)	0.000	0.015 (4)	0.000
N1	0.023 (2)	0.031 (2)	0.035 (2)	−0.0024 (17)	0.0090 (19)	0.0029 (18)
N2	0.029 (2)	0.032 (2)	0.043 (3)	0.0060 (18)	0.016 (2)	0.0032 (19)
N3	0.034 (3)	0.048 (3)	0.044 (3)	−0.016 (2)	0.010 (2)	0.000 (2)
N4	0.029 (2)	0.052 (3)	0.034 (2)	−0.007 (2)	0.007 (2)	0.000 (2)
O1	0.029 (2)	0.043 (2)	0.044 (2)	0.0123 (17)	0.0088 (19)	0.0045 (18)
O2	0.038 (2)	0.0322 (18)	0.035 (2)	0.0063 (16)	0.0155 (18)	0.0007 (15)
O1W	0.058 (3)	0.042 (2)	0.033 (2)	0.011 (2)	0.002 (2)	0.0042 (18)
O3	0.022 (2)	0.049 (2)	0.066 (3)	−0.0033 (17)	0.020 (2)	0.006 (2)
O4	0.051 (4)	0.032 (3)	0.062 (4)	0.000	0.035 (3)	0.000
O2W	0.057 (6)	0.059 (5)	0.119 (7)	0.000	−0.007 (5)	0.000
O5	0.049 (3)	0.048 (2)	0.058 (3)	−0.003 (2)	0.018 (2)	0.023 (2)
Cd1	0.02447 (19)	0.02697 (19)	0.0338 (2)	0.00214 (15)	0.01220 (15)	0.00352 (16)

Geometric parameters (Å, º)

top

C1—N1	1.333 (6)	C17—H17	0.9300
C1—C2	1.403 (7)	C18—N4	1.363 (7)
C1—H1	0.9300	C19—O1	1.240 (6)
C2—C3	1.370 (7)	C19—O2	1.265 (6)
C2—H2	0.9300	C19—C20	1.517 (6)
C3—C4	1.401 (7)	C19—Cd1	2.727 (5)
C3—H3	0.9300	C20—C26	1.378 (6)
C4—C5	1.386 (7)	C20—C22	1.389 (6)
C4—C6	1.478 (6)	C21—O3	1.236 (6)
C5—N1	1.365 (6)	C21—O5	1.252 (6)
C5—C9	1.455 (7)	C21—C22	1.526 (6)
C6—N4	1.335 (7)	C21—Cd1ⁱ	2.744 (5)
C6—C7	1.411 (7)	C22—C23	1.399 (6)
C7—N3	1.316 (6)	C23—C24	1.411 (6)
C7—C8	1.480 (7)	C23—H23	0.9300
C8—C11	1.392 (7)	C24—C25	1.385 (7)
C8—C9	1.395 (6)	C24—C27	1.489 (6)
C9—N2	1.356 (6)	C25—C26	1.400 (6)
C10—N2	1.328 (6)	C25—H25	0.9300
C10—C12	1.402 (8)	C26—H26	0.9300
C10—H10	0.9300	C27—O4	1.214 (9)
C11—C12	1.339 (9)	C27—C24ⁱⁱ	1.489 (6)
C11—H11	0.9300	Cd1—N1	2.352 (4)
C12—H12	0.9300	Cd1—N2	2.367 (4)
C13—N3	1.376 (8)	Cd1—O1	2.381 (4)
C13—C18	1.405 (9)	Cd1—O2	2.411 (3)
C13—C14	1.420 (8)	Cd1—O1W	2.323 (4)
C14—C15	1.374 (10)	O1W—HW11	0.84 (4)
C14—H14	0.9300	O1W—HW12	0.84 (4)
C15—C16	1.389 (10)	O2W—HW22	0.85 (2)
C15—H15	0.9300	O2W—HW21	0.85 (2)
C16—C17	1.381 (8)	Cd1—O3ⁱⁱⁱ	2.321 (4)
C16—H16	0.9300	Cd1—O5ⁱⁱⁱ	2.572 (4)
C17—C18	1.432 (8)

N1—C1—C2	123.1 (5)	C22—C20—C19	121.9 (4)
N1—C1—H1	118.5	O3—C21—O5	124.2 (5)
C2—C1—H1	118.5	O3—C21—C22	117.9 (5)
C3—C2—C1	118.7 (5)	O5—C21—C22	117.8 (5)
C3—C2—H2	120.6	O3—C21—Cd1ⁱ	57.2 (3)
C1—C2—H2	120.6	O5—C21—Cd1ⁱ	68.8 (3)
C2—C3—C4	119.0 (5)	C22—C21—Cd1ⁱ	162.6 (3)
C2—C3—H3	120.5	C20—C22—C23	120.1 (4)
C4—C3—H3	120.5	C20—C22—C21	122.3 (4)
C5—C4—C3	119.1 (4)	C23—C22—C21	117.4 (4)
C5—C4—C6	119.4 (4)	C22—C23—C24	120.4 (4)
C3—C4—C6	121.5 (5)	C22—C23—H23	119.8
N1—C5—C4	121.9 (4)	C24—C23—H23	119.8
N1—C5—C9	117.0 (4)	C25—C24—C23	118.4 (4)
C4—C5—C9	121.1 (4)	C25—C24—C27	124.4 (4)
N4—C6—C7	122.0 (4)	C23—C24—C27	117.1 (4)
N4—C6—C4	118.2 (5)	C24—C25—C26	120.5 (4)
C7—C6—C4	119.8 (4)	C24—C25—H25	119.7
N3—C7—C6	123.5 (5)	C26—C25—H25	119.7
N3—C7—C8	117.1 (5)	C20—C26—C25	120.8 (5)
C6—C7—C8	119.4 (4)	C20—C26—H26	119.6
C11—C8—C9	118.1 (5)	C25—C26—H26	119.6
C11—C8—C7	122.2 (4)	O4—C27—C24ⁱⁱ	120.1 (3)
C9—C8—C7	119.7 (5)	O4—C27—C24	120.1 (3)
N2—C9—C8	121.2 (5)	C24ⁱⁱ—C27—C24	119.7 (6)
N2—C9—C5	118.5 (4)	C1—N1—C5	118.1 (4)
C8—C9—C5	120.2 (5)	C1—N1—Cd1	124.5 (3)
N2—C10—C12	122.1 (5)	C5—N1—Cd1	117.2 (3)
N2—C10—H10	119.0	C10—N2—C9	119.1 (4)
C12—C10—H10	119.0	C10—N2—Cd1	124.5 (4)
C12—C11—C8	120.6 (5)	C9—N2—Cd1	116.3 (3)
C12—C11—H11	119.7	C7—N3—C13	115.5 (5)
C8—C11—H11	119.7	C6—N4—C18	115.4 (5)
C11—C12—C10	118.9 (5)	C19—O1—Cd1	92.2 (3)
C11—C12—H12	120.6	C19—O2—Cd1	90.2 (3)
C10—C12—H12	120.6	Cd1—O1W—HW11	123 (4)
N3—C13—C18	121.0 (5)	Cd1—O1W—HW12	117 (4)
N3—C13—C14	119.1 (6)	HW11—O1W—HW12	107 (3)
C18—C13—C14	119.9 (6)	C21—O3—Cd1ⁱ	96.2 (3)
C15—C14—C13	119.4 (7)	HW22—O2W—HW21	105 (3)
C15—C14—H14	120.3	C21—O5—Cd1ⁱ	84.2 (3)
C13—C14—H14	120.3	O3ⁱⁱⁱ—Cd1—O1W	102.56 (15)
C14—C15—C16	121.0 (6)	O3ⁱⁱⁱ—Cd1—N1	84.39 (13)
C14—C15—H15	119.5	O1W—Cd1—N1	102.54 (15)
C16—C15—H15	119.5	O3ⁱⁱⁱ—Cd1—N2	154.84 (14)
C17—C16—C15	121.6 (6)	O1W—Cd1—N2	82.23 (16)
C17—C16—H16	119.2	N1—Cd1—N2	70.49 (14)
C15—C16—H16	119.2	O3ⁱⁱⁱ—Cd1—O1	88.62 (13)
C16—C17—C18	118.6 (7)	O1W—Cd1—O1	153.69 (14)
C16—C17—H17	120.7	N1—Cd1—O1	102.20 (14)
C18—C17—H17	120.7	N2—Cd1—O1	97.78 (14)
N4—C18—C13	122.3 (5)	O3ⁱⁱⁱ—Cd1—O2	119.58 (12)
N4—C18—C17	118.0 (6)	O1W—Cd1—O2	99.59 (13)
C13—C18—C17	119.6 (5)	N1—Cd1—O2	142.59 (13)
O1—C19—O2	122.6 (4)	N2—Cd1—O2	83.19 (13)
O1—C19—C20	119.8 (5)	O1—Cd1—O2	54.58 (12)
O2—C19—C20	117.3 (4)	O3ⁱⁱⁱ—Cd1—O5ⁱⁱⁱ	53.13 (13)
O1—C19—Cd1	60.7 (3)	O1W—Cd1—O5ⁱⁱⁱ	82.76 (15)
O2—C19—Cd1	62.2 (2)	N1—Cd1—O5ⁱⁱⁱ	136.94 (13)
C20—C19—Cd1	167.9 (3)	N2—Cd1—O5ⁱⁱⁱ	151.32 (14)
C26—C20—C22	119.5 (4)	O1—Cd1—O5ⁱⁱⁱ	85.29 (13)
C26—C20—C19	118.2 (4)	O2—Cd1—O5ⁱⁱⁱ	75.40 (12)

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

Hydrogen-bond geometry (Å, º)

top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—HW11···O2^iv	0.84 (4)	1.92 (3)	2.731 (5)	163 (6)
O1W—HW12···O5^iv	0.84 (4)	2.23 (4)	2.892 (6)	136 (5)
O2W—HW22···O1ⁱⁱⁱ	0.85 (2)	2.14 (8)	2.913 (5)	152 (15)

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

Experimental details

Crystal data
Chemical formula	[Cd₂(C₁₇H₆O₉)(C₁₈H₁₀N₄)₂(H₂O)₂]·H₂O
M_r	1197.67
Crystal system, space group	Monoclinic, P2/n
Temperature (K)	293
a, b, c (Å)	15.698 (3), 6.7028 (13), 21.428 (4)
β (°)	102.45 (3)
V (Å³)	2201.7 (8)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.05
Crystal size (mm)	0.27 × 0.24 × 0.21

Data collection
Diffractometer	Rigaku R-AXIS RAPID diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.742, 0.801
No. of measured, independent and observed [I > 2σ(I)] reflections	20222, 5022, 3508
R_int	0.093
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.049, 0.125, 1.04
No. of reflections	5022
No. of parameters	352
No. of restraints	6
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.70, −0.84

Computer programs: PROCESS-AUTO (Rigaku, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL-Plus (Sheldrick, 2008).

Selected geometric parameters (Å, º)

top

Cd1—N1	2.352 (4)	Cd1—O1W	2.323 (4)
Cd1—N2	2.367 (4)	Cd1—O3ⁱ	2.321 (4)
Cd1—O1	2.381 (4)	Cd1—O5ⁱ	2.572 (4)
Cd1—O2	2.411 (3)

O3ⁱ—Cd1—O1W	102.56 (15)	O1W—Cd1—O2	99.59 (13)
O3ⁱ—Cd1—N1	84.39 (13)	N1—Cd1—O2	142.59 (13)
O1W—Cd1—N1	102.54 (15)	N2—Cd1—O2	83.19 (13)
O3ⁱ—Cd1—N2	154.84 (14)	O1—Cd1—O2	54.58 (12)
O1W—Cd1—N2	82.23 (16)	O3ⁱ—Cd1—O5ⁱ	53.13 (13)
N1—Cd1—N2	70.49 (14)	O1W—Cd1—O5ⁱ	82.76 (15)
O3ⁱ—Cd1—O1	88.62 (13)	N1—Cd1—O5ⁱ	136.94 (13)
O1W—Cd1—O1	153.69 (14)	N2—Cd1—O5ⁱ	151.32 (14)
N1—Cd1—O1	102.20 (14)	O1—Cd1—O5ⁱ	85.29 (13)
N2—Cd1—O1	97.78 (14)	O2—Cd1—O5ⁱ	75.40 (12)
O3ⁱ—Cd1—O2	119.58 (12)

Symmetry code: (i) x, y−1, z.

Hydrogen-bond geometry (Å, º)

top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—HW11···O2ⁱⁱ	0.84(4)	1.92(3)	2.731(5)	163(6)
O1W—HW12···O5ⁱⁱ	0.84(4)	2.23(4)	2.892(6)	136(5)
O2W—HW22···O1ⁱ	0.85(2)	2.14(8)	2.913(5)	152(15)

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

Acknowledgements

This work was supported by the Program for Young Academic Backbone in Heilongjiang Provincial University (No. 1152 G053) and Mudanjiang Medical University.

References

Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. GoogleScholar
Li, C.-B., Fang, W., Dong, E.-J., Liu, B. & Li, Y.-W. (2007). Acta Cryst. E63, m150–m152. WebofScience CSD CrossRef IUCrJournals GoogleScholar
Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan. GoogleScholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. WebofScience CrossRef CAS IUCrJournals GoogleScholar
Wu, J.-Z., Li, L., Zeng, T.-X., Ji, L.-N., Zhou, J.-Y., Luo, T. & Li, R.-H. (1997). Polyhedron, 16, 103–107. CrossRef CAS WebofScience GoogleScholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 64| Part 6| June 2008| Pagesm810-m811

doi:10.1107/S1600536808013676

Openaccess

Poly[[diaqua­[μ4-4,4′-carbonyl­bis(benzene-1,2-dicarboxyl­ato)]bis­(dipyrido[3,2-a:2′,3′-c]phenazine)dicadmium(II)] monohydrate] (2024)

metal-organic compounds