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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 64| Part 6| June 2008| Pages m810-m811

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

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 CdII 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 CdII 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[Li, C.-B., Fang, W., Dong, E.-J., Liu, B. & Li, Y.-W. (2007). Acta Cryst. E63, m150-m152.]); Wu et al. (1997[Wu, J.-Z., Li, L., Zeng, T.-X., Ji, L.-N., Zhou, J.-Y., Luo, T. & Li, R.-H. (1997). Polyhedron, 16, 103-107.]).

[Scheme 1]

Experimental

Crystal data
  • [Cd2(C17H6O9)(C18H10N4)2(H2O)2]·H2O

  • Mr = 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[Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.742, Tmax = 0.801

  • 20222 measured reflections

  • 5022 independent reflections

  • 3508 reflections with I > 2σ(I)

  • Rint = 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

  • Δρmax = 0.70 e Å−3

  • Δρmin = −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 DA 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[Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan.]); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL-Plus (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXL97.

Supporting information


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 CdII 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 CdII 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 ππ 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 Uiso(H) = 1.2Ueq(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 Uiso(H) = 1.2Ueq(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
[Figure 1] 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.
[Figure 2] 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]·H2OF(000) = 1196
Mr = 1197.67Dx = 1.807 Mg m3
Monoclinic, P2/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yacCell parameters from 13844 reflections
a = 15.698 (3) Åθ = 3.0–27.5°
b = 6.7028 (13) ŵ = 1.05 mm1
c = 21.428 (4) ÅT = 293 K
β = 102.45 (3)°Block, colourless
V = 2201.7 (8) Å30.27 × 0.24 × 0.21 mm
Z = 2
Data collection top
Rigaku R-AXIS RAPID
diffractometer
5022 independent reflections
Radiation source: rotating anode3508 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.093
Detector resolution: 10.0 pixels mm-1θmax = 27.5°, θmin = 3.0°
ω scansh = 2018
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 88
Tmin = 0.742, Tmax = 0.801l = 2727
20222 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.049Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.125H atoms treated by a mixture of independent and constrained refinement
S = 1.04 w = 1/[σ2(Fo2) + (0.0614P)2]
where P = (Fo2 + 2Fc2)/3
5022 reflections(Δ/σ)max < 0.001
352 parametersΔρmax = 0.70 e Å3
6 restraintsΔρmin = 0.84 e Å3
Crystal data top
[Cd2(C17H6O9)(C18H10N4)2(H2O)2]·H2OV = 2201.7 (8) Å3
Mr = 1197.67Z = 2
Monoclinic, P2/nMo Kα radiation
a = 15.698 (3) ŵ = 1.05 mm1
b = 6.7028 (13) ÅT = 293 K
c = 21.428 (4) Å0.27 × 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)
Tmin = 0.742, Tmax = 0.801Rint = 0.093
20222 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0496 restraints
wR(F2) = 0.125H atoms treated by a mixture of independent and constrained refinement
S = 1.04Δρmax = 0.70 e Å3
5022 reflectionsΔρmin = 0.84 e Å3
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
xyzUiso*/UeqOcc. (<1)
C10.7768 (4)0.0149 (8)0.1740 (2)0.0342 (12)
H10.73430.06380.18610.041*
C20.8642 (3)0.0462 (8)0.1917 (3)0.0377 (13)
H20.87940.15970.21660.045*
C30.9266 (4)0.0645 (8)0.1717 (3)0.0367 (12)
H30.98480.02550.18190.044*
C40.9015 (3)0.2375 (7)0.1356 (2)0.0286 (11)
C50.8145 (3)0.2937 (7)0.1223 (2)0.0261 (10)
C60.9661 (3)0.3643 (8)0.1135 (2)0.0319 (11)
C70.9401 (4)0.5492 (8)0.0840 (2)0.0339 (12)
C80.8467 (4)0.6054 (7)0.0703 (2)0.0316 (12)
C90.7859 (3)0.4772 (7)0.0878 (2)0.0281 (11)
C100.6728 (4)0.6892 (8)0.0431 (3)0.0423 (14)
H100.61340.71740.03280.051*
C110.8165 (4)0.7825 (8)0.0393 (3)0.0398 (13)
H110.85590.87160.02790.048*
C120.7312 (4)0.8258 (8)0.0259 (3)0.0502 (17)
H120.71120.94460.00550.060*
C131.0803 (4)0.6155 (10)0.0777 (3)0.0455 (15)
C141.1439 (5)0.7468 (10)0.0625 (3)0.0604 (19)
H141.12800.87370.04660.072*
C151.2290 (5)0.6847 (13)0.0715 (3)0.068 (2)
H151.27080.77070.06180.082*
C161.2537 (4)0.4954 (12)0.0950 (3)0.0566 (19)
H161.31160.45620.09980.068*
C171.1943 (4)0.3640 (12)0.1113 (3)0.0550 (17)
H171.21190.23830.12750.066*
C181.1052 (4)0.4256 (9)0.1028 (3)0.0395 (13)
C190.5216 (3)0.5601 (7)0.1603 (3)0.0300 (11)
C200.4599 (3)0.6828 (7)0.1904 (2)0.0250 (10)
C210.4935 (3)1.0024 (7)0.1355 (2)0.0298 (11)
C220.4394 (3)0.8792 (7)0.1726 (2)0.0228 (10)
C230.3716 (3)0.9765 (7)0.1933 (2)0.0264 (10)
H230.35851.10840.18170.032*
C240.3230 (3)0.8755 (7)0.2318 (2)0.0270 (11)
C250.3484 (3)0.6844 (7)0.2525 (2)0.0320 (12)
H250.32010.61920.28050.038*
C260.4164 (3)0.5886 (7)0.2315 (2)0.0311 (11)
H260.43240.45980.24540.037*
C270.25000.9870 (11)0.25000.0338 (17)
N10.7518 (3)0.1804 (6)0.1405 (2)0.0292 (9)
N20.6995 (3)0.5206 (6)0.0737 (2)0.0333 (10)
N30.9946 (3)0.6766 (7)0.0669 (2)0.0419 (11)
N41.0483 (3)0.2994 (7)0.1226 (2)0.0385 (11)
O10.5763 (2)0.4504 (5)0.19432 (18)0.0386 (9)
O20.5089 (2)0.5605 (5)0.09996 (17)0.0338 (8)
O1W0.5801 (3)0.2021 (6)0.00419 (19)0.0457 (10)
HW110.563 (4)0.287 (6)0.033 (2)0.055*
HW120.553 (3)0.096 (5)0.016 (3)0.055*
O30.5736 (2)0.9818 (6)0.1491 (2)0.0443 (10)
O40.25001.1681 (8)0.25000.0448 (15)
O2W0.75000.3982 (12)0.25000.082 (2)
HW220.708 (7)0.479 (19)0.240 (8)0.099*0.50
HW210.764 (14)0.40 (2)0.2906 (11)0.099*0.50
O50.4540 (3)1.1233 (6)0.0948 (2)0.0506 (11)
Cd10.60585 (2)0.27952 (5)0.103914 (18)0.02753 (13)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.034 (3)0.038 (3)0.032 (3)0.002 (2)0.010 (3)0.007 (2)
C20.033 (3)0.039 (3)0.040 (3)0.003 (2)0.006 (3)0.013 (2)
C30.029 (3)0.043 (3)0.035 (3)0.001 (2)0.001 (3)0.005 (2)
C40.028 (3)0.031 (3)0.028 (2)0.001 (2)0.008 (2)0.004 (2)
C50.025 (2)0.030 (2)0.026 (2)0.000 (2)0.011 (2)0.002 (2)
C60.024 (3)0.043 (3)0.030 (3)0.009 (2)0.009 (2)0.000 (2)
C70.035 (3)0.037 (3)0.032 (3)0.012 (2)0.013 (3)0.005 (2)
C80.036 (3)0.031 (3)0.031 (3)0.009 (2)0.014 (3)0.000 (2)
C90.030 (3)0.025 (2)0.031 (3)0.003 (2)0.010 (2)0.000 (2)
C100.036 (3)0.038 (3)0.058 (4)0.010 (2)0.020 (3)0.011 (3)
C110.046 (3)0.030 (3)0.046 (3)0.003 (2)0.016 (3)0.005 (2)
C120.063 (4)0.028 (3)0.065 (4)0.008 (3)0.026 (4)0.018 (3)
C130.034 (3)0.066 (4)0.036 (3)0.023 (3)0.008 (3)0.008 (3)
C140.051 (4)0.073 (5)0.061 (4)0.024 (4)0.021 (4)0.009 (3)
C150.041 (4)0.110 (6)0.056 (4)0.039 (4)0.018 (4)0.002 (4)
C160.023 (3)0.108 (6)0.042 (4)0.019 (3)0.013 (3)0.011 (4)
C170.033 (3)0.095 (5)0.038 (3)0.007 (3)0.008 (3)0.001 (3)
C180.024 (3)0.065 (4)0.030 (3)0.010 (3)0.008 (2)0.003 (3)
C190.027 (3)0.027 (2)0.040 (3)0.002 (2)0.015 (3)0.002 (2)
C200.015 (2)0.032 (3)0.029 (2)0.0024 (18)0.005 (2)0.001 (2)
C210.033 (3)0.028 (3)0.031 (3)0.005 (2)0.013 (2)0.004 (2)
C220.014 (2)0.029 (2)0.025 (2)0.0026 (18)0.004 (2)0.0002 (19)
C230.023 (3)0.028 (2)0.030 (3)0.0025 (19)0.009 (2)0.002 (2)
C240.020 (2)0.033 (3)0.031 (3)0.004 (2)0.013 (2)0.002 (2)
C250.032 (3)0.033 (3)0.035 (3)0.005 (2)0.015 (2)0.004 (2)
C260.027 (3)0.030 (2)0.036 (3)0.002 (2)0.007 (2)0.005 (2)
C270.036 (4)0.038 (4)0.030 (4)0.0000.015 (4)0.000
N10.023 (2)0.031 (2)0.035 (2)0.0024 (17)0.0090 (19)0.0029 (18)
N20.029 (2)0.032 (2)0.043 (3)0.0060 (18)0.016 (2)0.0032 (19)
N30.034 (3)0.048 (3)0.044 (3)0.016 (2)0.010 (2)0.000 (2)
N40.029 (2)0.052 (3)0.034 (2)0.007 (2)0.007 (2)0.000 (2)
O10.029 (2)0.043 (2)0.044 (2)0.0123 (17)0.0088 (19)0.0045 (18)
O20.038 (2)0.0322 (18)0.035 (2)0.0063 (16)0.0155 (18)0.0007 (15)
O1W0.058 (3)0.042 (2)0.033 (2)0.011 (2)0.002 (2)0.0042 (18)
O30.022 (2)0.049 (2)0.066 (3)0.0033 (17)0.020 (2)0.006 (2)
O40.051 (4)0.032 (3)0.062 (4)0.0000.035 (3)0.000
O2W0.057 (6)0.059 (5)0.119 (7)0.0000.007 (5)0.000
O50.049 (3)0.048 (2)0.058 (3)0.003 (2)0.018 (2)0.023 (2)
Cd10.02447 (19)0.02697 (19)0.0338 (2)0.00214 (15)0.01220 (15)0.00352 (16)
Geometric parameters (Å, º) top
C1—N11.333 (6)C17—H170.9300
C1—C21.403 (7)C18—N41.363 (7)
C1—H10.9300C19—O11.240 (6)
C2—C31.370 (7)C19—O21.265 (6)
C2—H20.9300C19—C201.517 (6)
C3—C41.401 (7)C19—Cd12.727 (5)
C3—H30.9300C20—C261.378 (6)
C4—C51.386 (7)C20—C221.389 (6)
C4—C61.478 (6)C21—O31.236 (6)
C5—N11.365 (6)C21—O51.252 (6)
C5—C91.455 (7)C21—C221.526 (6)
C6—N41.335 (7)C21—Cd1i2.744 (5)
C6—C71.411 (7)C22—C231.399 (6)
C7—N31.316 (6)C23—C241.411 (6)
C7—C81.480 (7)C23—H230.9300
C8—C111.392 (7)C24—C251.385 (7)
C8—C91.395 (6)C24—C271.489 (6)
C9—N21.356 (6)C25—C261.400 (6)
C10—N21.328 (6)C25—H250.9300
C10—C121.402 (8)C26—H260.9300
C10—H100.9300C27—O41.214 (9)
C11—C121.339 (9)C27—C24ii1.489 (6)
C11—H110.9300Cd1—N12.352 (4)
C12—H120.9300Cd1—N22.367 (4)
C13—N31.376 (8)Cd1—O12.381 (4)
C13—C181.405 (9)Cd1—O22.411 (3)
C13—C141.420 (8)Cd1—O1W2.323 (4)
C14—C151.374 (10)O1W—HW110.84 (4)
C14—H140.9300O1W—HW120.84 (4)
C15—C161.389 (10)O2W—HW220.85 (2)
C15—H150.9300O2W—HW210.85 (2)
C16—C171.381 (8)Cd1—O3iii2.321 (4)
C16—H160.9300Cd1—O5iii2.572 (4)
C17—C181.432 (8)
N1—C1—C2123.1 (5)C22—C20—C19121.9 (4)
N1—C1—H1118.5O3—C21—O5124.2 (5)
C2—C1—H1118.5O3—C21—C22117.9 (5)
C3—C2—C1118.7 (5)O5—C21—C22117.8 (5)
C3—C2—H2120.6O3—C21—Cd1i57.2 (3)
C1—C2—H2120.6O5—C21—Cd1i68.8 (3)
C2—C3—C4119.0 (5)C22—C21—Cd1i162.6 (3)
C2—C3—H3120.5C20—C22—C23120.1 (4)
C4—C3—H3120.5C20—C22—C21122.3 (4)
C5—C4—C3119.1 (4)C23—C22—C21117.4 (4)
C5—C4—C6119.4 (4)C22—C23—C24120.4 (4)
C3—C4—C6121.5 (5)C22—C23—H23119.8
N1—C5—C4121.9 (4)C24—C23—H23119.8
N1—C5—C9117.0 (4)C25—C24—C23118.4 (4)
C4—C5—C9121.1 (4)C25—C24—C27124.4 (4)
N4—C6—C7122.0 (4)C23—C24—C27117.1 (4)
N4—C6—C4118.2 (5)C24—C25—C26120.5 (4)
C7—C6—C4119.8 (4)C24—C25—H25119.7
N3—C7—C6123.5 (5)C26—C25—H25119.7
N3—C7—C8117.1 (5)C20—C26—C25120.8 (5)
C6—C7—C8119.4 (4)C20—C26—H26119.6
C11—C8—C9118.1 (5)C25—C26—H26119.6
C11—C8—C7122.2 (4)O4—C27—C24ii120.1 (3)
C9—C8—C7119.7 (5)O4—C27—C24120.1 (3)
N2—C9—C8121.2 (5)C24ii—C27—C24119.7 (6)
N2—C9—C5118.5 (4)C1—N1—C5118.1 (4)
C8—C9—C5120.2 (5)C1—N1—Cd1124.5 (3)
N2—C10—C12122.1 (5)C5—N1—Cd1117.2 (3)
N2—C10—H10119.0C10—N2—C9119.1 (4)
C12—C10—H10119.0C10—N2—Cd1124.5 (4)
C12—C11—C8120.6 (5)C9—N2—Cd1116.3 (3)
C12—C11—H11119.7C7—N3—C13115.5 (5)
C8—C11—H11119.7C6—N4—C18115.4 (5)
C11—C12—C10118.9 (5)C19—O1—Cd192.2 (3)
C11—C12—H12120.6C19—O2—Cd190.2 (3)
C10—C12—H12120.6Cd1—O1W—HW11123 (4)
N3—C13—C18121.0 (5)Cd1—O1W—HW12117 (4)
N3—C13—C14119.1 (6)HW11—O1W—HW12107 (3)
C18—C13—C14119.9 (6)C21—O3—Cd1i96.2 (3)
C15—C14—C13119.4 (7)HW22—O2W—HW21105 (3)
C15—C14—H14120.3C21—O5—Cd1i84.2 (3)
C13—C14—H14120.3O3iii—Cd1—O1W102.56 (15)
C14—C15—C16121.0 (6)O3iii—Cd1—N184.39 (13)
C14—C15—H15119.5O1W—Cd1—N1102.54 (15)
C16—C15—H15119.5O3iii—Cd1—N2154.84 (14)
C17—C16—C15121.6 (6)O1W—Cd1—N282.23 (16)
C17—C16—H16119.2N1—Cd1—N270.49 (14)
C15—C16—H16119.2O3iii—Cd1—O188.62 (13)
C16—C17—C18118.6 (7)O1W—Cd1—O1153.69 (14)
C16—C17—H17120.7N1—Cd1—O1102.20 (14)
C18—C17—H17120.7N2—Cd1—O197.78 (14)
N4—C18—C13122.3 (5)O3iii—Cd1—O2119.58 (12)
N4—C18—C17118.0 (6)O1W—Cd1—O299.59 (13)
C13—C18—C17119.6 (5)N1—Cd1—O2142.59 (13)
O1—C19—O2122.6 (4)N2—Cd1—O283.19 (13)
O1—C19—C20119.8 (5)O1—Cd1—O254.58 (12)
O2—C19—C20117.3 (4)O3iii—Cd1—O5iii53.13 (13)
O1—C19—Cd160.7 (3)O1W—Cd1—O5iii82.76 (15)
O2—C19—Cd162.2 (2)N1—Cd1—O5iii136.94 (13)
C20—C19—Cd1167.9 (3)N2—Cd1—O5iii151.32 (14)
C26—C20—C22119.5 (4)O1—Cd1—O5iii85.29 (13)
C26—C20—C19118.2 (4)O2—Cd1—O5iii75.40 (12)
Symmetry codes: (i) x, y+1, z; (ii) x+1/2, y, z+1/2; (iii) x, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—HW11···O2iv0.84 (4)1.92 (3)2.731 (5)163 (6)
O1W—HW12···O5iv0.84 (4)2.23 (4)2.892 (6)136 (5)
O2W—HW22···O1iii0.85 (2)2.14 (8)2.913 (5)152 (15)
Symmetry codes: (iii) x, y1, z; (iv) x+1, y+1, z.

Experimental details

Crystal data
Chemical formula[Cd2(C17H6O9)(C18H10N4)2(H2O)2]·H2O
Mr1197.67
Crystal system, space groupMonoclinic, P2/n
Temperature (K)293
a, b, c (Å)15.698 (3), 6.7028 (13), 21.428 (4)
β (°) 102.45 (3)
V3)2201.7 (8)
Z2
Radiation typeMo Kα
µ (mm1)1.05
Crystal size (mm)0.27 × 0.24 × 0.21
Data collection
DiffractometerRigaku R-AXIS RAPID
diffractometer
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.742, 0.801
No. of measured, independent and
observed [I > 2σ(I)] reflections
20222, 5022, 3508
Rint0.093
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.049, 0.125, 1.04
No. of reflections5022
No. of parameters352
No. of restraints6
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)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—N12.352 (4)Cd1—O1W2.323 (4)
Cd1—N22.367 (4)Cd1—O3i2.321 (4)
Cd1—O12.381 (4)Cd1—O5i2.572 (4)
Cd1—O22.411 (3)
O3i—Cd1—O1W102.56 (15)O1W—Cd1—O299.59 (13)
O3i—Cd1—N184.39 (13)N1—Cd1—O2142.59 (13)
O1W—Cd1—N1102.54 (15)N2—Cd1—O283.19 (13)
O3i—Cd1—N2154.84 (14)O1—Cd1—O254.58 (12)
O1W—Cd1—N282.23 (16)O3i—Cd1—O5i53.13 (13)
N1—Cd1—N270.49 (14)O1W—Cd1—O5i82.76 (15)
O3i—Cd1—O188.62 (13)N1—Cd1—O5i136.94 (13)
O1W—Cd1—O1153.69 (14)N2—Cd1—O5i151.32 (14)
N1—Cd1—O1102.20 (14)O1—Cd1—O5i85.29 (13)
N2—Cd1—O197.78 (14)O2—Cd1—O5i75.40 (12)
O3i—Cd1—O2119.58 (12)
Symmetry code: (i) x, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—HW11···O2ii0.84 (4)1.92 (3)2.731 (5)163 (6)
O1W—HW12···O5ii0.84 (4)2.23 (4)2.892 (6)136 (5)
O2W—HW22···O1i0.85 (2)2.14 (8)2.913 (5)152 (15)
Symmetry codes: (i) x, y1, 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

First citationHigashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.  Google Scholar
First citationLi, C.-B., Fang, W., Dong, E.-J., Liu, B. & Li, Y.-W. (2007). Acta Cryst. E63, m150–m152.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationRigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationWu, 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 Web of Science Google Scholar

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Volume 64| Part 6| June 2008| Pages m810-m811
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