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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

catena-Poly[[[bis­­[μ-3-(4-carb­­oxy­phen­­oxy)propionato]-κ3O1,O1′:O1;κ3O1:O1,O1′-bis­­[aqua­(N,N-di­methyl­formamide-κO)cadmium]]-μ-4,4′-bi­pyridine-κ2N:N′] dinitrate]

aKey Laboratory of Functional Inorganic Materials Chemistry, Ministry of Education, Heilongjiang University, Harbin 150080, People's Republic of China, bDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia, and cChemistry Department, Faculty of Science, King Abdulaziz University, PO Box 80203 Jeddah, Saudi Arabia
*Correspondence e-mail: seikweng@um.edu.my

(Received 24 January 2012; accepted 24 January 2012; online 31 January 2012)

In the title coordination polymer, {[Cd2(C10H9O5)2(C10H8N2)2(C3H7NO)2(H2O)2](NO3)2}n, the 3-(4-carb­oxy­phen­oxy)propionate monoanion O,O′-chelates to a CdII cation through the aliphatic carboxyl­ate end. One of these O atoms is also connected to the metal cation from an inversion-related metal atom. The five O atoms bonded to the metal centre form a penta­gon, above and below which are located the N atoms of the 4,4′-bipyridine mol­ecules. The polycationic ribbon propagates along the b axis of the unit cell. The (aromatic) carboxyl end of the monoanion connects adjacent ribbons into a layer motif in the (102) plane. The nitrate ions are hydrogen bonded to the layer. The geometry of the CdII atom is a trans-N2O5Cd penta­gonal bipyramid.

Related literature

For 3-(4-carb­oxy­phen­oxy)propionic acid, see: Gao & Ng (2006[Gao, S. & Ng, S. W. (2006). Acta Cryst. E62, o3420-o3421.]).

[Scheme 1]

Experimental

Crystal data
  • [Cd2(C10H9O5)2(C10H8N2)2(C3H7NO)2(H2O)2](NO3)2

  • Mr = 1261.76

  • Triclinic, [P \overline 1]

  • a = 9.1020 (5) Å

  • b = 11.6866 (5) Å

  • c = 13.3534 (5) Å

  • α = 69.1646 (11)°

  • β = 84.2052 (16)°

  • γ = 76.9358 (16)°

  • V = 1292.84 (10) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 0.91 mm−1

  • T = 293 K

  • 0.19 × 0.12 × 0.11 mm

Data collection
  • Rigaku R-AXIS RAPID IP diffractometer

  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995[Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.847, Tmax = 0.907

  • 12594 measured reflections

  • 5822 independent reflections

  • 4760 reflections with I > 2σ(I)

  • Rint = 0.031

Refinement
  • R[F2 > 2σ(F2)] = 0.030

  • wR(F2) = 0.077

  • S = 1.08

  • 5822 reflections

  • 345 parameters

  • H-atom parameters constrained

  • Δρmax = 0.95 e Å−3

  • Δρmin = −0.59 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O5—H5⋯O4i 0.84 1.80 2.629 (3) 171
O1W—H11⋯O7 0.84 1.94 2.754 (4) 164
O1W—H12⋯O2ii 0.84 2.03 2.763 (3) 145
Symmetry codes: (i) -x+2, -y+1, -z; (ii) -x+1, -y+2, -z+1.

Data collection: RAPID-AUTO (Rigaku, 1998[Rigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.]); cell refinement: RAPID-AUTO; data reduction: CrystalClear (Rigaku, 2002[Rigaku (2002). CrystalClear. Rigaku/MSC Inc., The Woodlands, Texas, USA.]); 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: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supporting information


Comment top

We reported the crystal structure of 3-(4-carboxyphenoxy)propropionic acid (Gao & Ng, 2006). We also reported the crystal structures of some metal derivatives. In the coordination polymer, [Cd2(H2O)2(C10H8N2)2(DMF)2(C10H8O5)2]n 2n(NO3) (Scheme I), the 3-(4-carboxyphenoxy)propionate monoanion O,O'-chelates to a CdII atom atom through the aliphatic (negatively-charged) carboxyl –CO2 end; one of the O atoms is also connected to an inversion-related metal atom. The carboxyl O atoms, the carboxyl O atom of an inversion-related dianion, and the O atoms of the water and DMF molecules comprise a pentagon, above and below which are located the N atoms of the 4,4'-bipyridine heterocycle (Fig. 1). The polycationic ribbon propogates along the b-axis of the unit cell; the (aromatic) carboxylic acid end of the monoanion connects adjacent ribbons (Fig. 2) into a layer motif; the nitrate ions are hydrogen bonded to the layer (Table 1).

Related literature top

For 3-(4-carboxyphenoxy)propropionic acid, see: Gao & Ng (2006).

Experimental top

Cadmium nitrate and 3-(4-carboxyphenoxy)propionic acid (1 mmol) were mixed in a water-DMF (3/1) mixture (10 ml). 4,4'-Bipyridine dissolved in methanol (5 ml) was added. The mixture was stirred until the reactants dissolved. Yellow crystals were isolated after a few days.

Refinement top

Carbon-bound H-atoms were placed in calculated positions (C–H 0.93–0.97 Å) and were included in the refinement in the riding model approximation, with U(H) set to 1.2–1.5U(C). The acid and water H-atoms were similarly treated (O–H 0.84 Å) and their displacement parameters were similarly tied.

Omitted owing to bad disagreement, the (0 2 0), (10 2 8), (9 2 11), (4 0 13), (4 - 1 14), (1 - 1 14), (10 4 9), (3 - 2 13), (2 - 2 13), (9 3 11), (10 2 9) and (10 5 10) reflections were omitted from refinement.

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); data reduction: CrystalClear (Rigaku, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. Anitoropic displacement ellipsoid plot (Barbour, 2001) of a portion of polymeric [Cd2(H2O)2(C10H8N2)2(C3H7NO)2(C10H8O5)2]n 2n(NO3) at the 50% probability level; hydrogen atoms are drawn as spheres of arbitrary radius.
[Figure 2] Fig. 2. Polycationic ribbon motif.
catena-Poly[[[bis[µ-3-(4-carboxyphenoxy)propionato]- κ3O1,O1':O1; κ3O1:O1,O1'- bis[aqua(N,N-dimethylformamide-κO)cadmium]]-µ- 4,4'-bipyridine-κ2N:N'] dinitrate] top
Crystal data top
[Cd2(C10H9O5)2(C10H8N2)2(C3H7NO)2(H2O)2](NO3)2Z = 1
Mr = 1261.76F(000) = 640
Triclinic, P1Dx = 1.621 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.1020 (5) ÅCell parameters from 10397 reflections
b = 11.6866 (5) Åθ = 3.2–27.5°
c = 13.3534 (5) ŵ = 0.91 mm1
α = 69.1646 (11)°T = 293 K
β = 84.2052 (16)°Prism, yellow
γ = 76.9358 (16)°0.19 × 0.12 × 0.11 mm
V = 1292.84 (10) Å3
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
5822 independent reflections
Radiation source: fine-focus sealed tube4760 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
ω scanθmax = 27.5°, θmin = 3.2°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 1111
Tmin = 0.847, Tmax = 0.907k = 1514
12594 measured reflectionsl = 1716
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)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.077H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.0367P)2 + 0.2058P]
where P = (Fo2 + 2Fc2)/3
5822 reflections(Δ/σ)max = 0.001
345 parametersΔρmax = 0.95 e Å3
0 restraintsΔρmin = 0.59 e Å3
Crystal data top
[Cd2(C10H9O5)2(C10H8N2)2(C3H7NO)2(H2O)2](NO3)2γ = 76.9358 (16)°
Mr = 1261.76V = 1292.84 (10) Å3
Triclinic, P1Z = 1
a = 9.1020 (5) ÅMo Kα radiation
b = 11.6866 (5) ŵ = 0.91 mm1
c = 13.3534 (5) ÅT = 293 K
α = 69.1646 (11)°0.19 × 0.12 × 0.11 mm
β = 84.2052 (16)°
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
5822 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
4760 reflections with I > 2σ(I)
Tmin = 0.847, Tmax = 0.907Rint = 0.031
12594 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0300 restraints
wR(F2) = 0.077H-atom parameters constrained
S = 1.08Δρmax = 0.95 e Å3
5822 reflectionsΔρmin = 0.59 e Å3
345 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cd10.18002 (2)0.944005 (16)0.589093 (15)0.02562 (7)
O10.0904 (2)1.01688 (18)0.40717 (15)0.0361 (4)
O20.3311 (2)1.00556 (19)0.41763 (15)0.0390 (5)
O30.3901 (3)0.8936 (2)0.23010 (18)0.0493 (6)
O40.8546 (3)0.4867 (2)0.0878 (2)0.0620 (7)
O50.9522 (3)0.6549 (2)0.0014 (2)0.0741 (8)
H51.01930.61530.02880.111*
O60.1426 (3)0.8763 (2)0.77857 (16)0.0479 (5)
O70.5403 (4)0.6153 (3)0.6982 (3)0.0893 (10)
O80.7250 (5)0.6396 (4)0.7677 (4)0.1299 (16)
O90.7435 (3)0.4764 (3)0.7307 (3)0.0829 (9)
O1W0.4333 (2)0.8691 (2)0.64542 (17)0.0486 (5)
H110.46110.79410.64930.073*
H120.48900.91240.60100.073*
N10.1779 (3)0.74731 (19)0.58879 (18)0.0307 (5)
N20.1773 (3)0.1380 (2)0.59570 (18)0.0315 (5)
N30.2606 (4)0.7602 (3)0.9348 (2)0.0646 (9)
N40.6706 (4)0.5765 (3)0.7332 (3)0.0596 (8)
C10.2171 (3)1.0305 (2)0.3627 (2)0.0282 (5)
C20.2299 (4)1.0791 (3)0.2418 (2)0.0423 (7)
H2A0.21581.16950.21700.051*
H2B0.14971.05860.21300.051*
C30.3801 (4)1.0261 (3)0.1987 (2)0.0440 (7)
H3A0.38531.06340.12130.053*
H3B0.46241.04310.22840.053*
C40.5115 (4)0.8267 (3)0.1927 (2)0.0413 (7)
C50.5131 (4)0.7005 (3)0.2196 (2)0.0426 (7)
H5A0.43730.66570.26390.051*
C60.6268 (4)0.6263 (3)0.1807 (2)0.0412 (7)
H60.62750.54160.19900.049*
C70.7403 (4)0.6773 (3)0.1143 (2)0.0415 (7)
C80.7405 (4)0.8018 (3)0.0913 (3)0.0515 (8)
H80.81780.83600.04850.062*
C90.6276 (4)0.8772 (3)0.1307 (3)0.0514 (8)
H90.62990.96080.11560.062*
C100.8552 (4)0.5984 (3)0.0665 (3)0.0481 (8)
C110.0810 (3)0.6805 (2)0.6513 (2)0.0339 (6)
H11A0.01480.71500.69570.041*
C120.0742 (3)0.5627 (2)0.6532 (2)0.0330 (6)
H12A0.00440.51980.69780.040*
C130.1722 (3)0.5090 (2)0.5881 (2)0.0279 (5)
C140.2714 (3)0.5799 (2)0.5215 (2)0.0366 (6)
H140.33760.54860.47520.044*
C150.2709 (3)0.6963 (3)0.5248 (2)0.0362 (6)
H150.33850.74190.48020.043*
C160.0616 (3)0.2007 (3)0.6371 (2)0.0376 (7)
H160.01880.16220.66810.045*
C170.0552 (3)0.3203 (3)0.6364 (2)0.0381 (7)
H170.02820.36050.66610.046*
C180.1735 (3)0.3800 (2)0.5914 (2)0.0278 (5)
C190.2945 (4)0.3138 (3)0.5491 (3)0.0428 (7)
H190.37680.34980.51800.051*
C200.2921 (4)0.1946 (3)0.5536 (3)0.0448 (8)
H200.37480.15150.52580.054*
C210.2327 (4)0.7857 (3)0.8328 (3)0.0483 (8)
H210.28580.73040.79980.058*
C220.1831 (6)0.8376 (5)0.9937 (4)0.0898 (16)
H22A0.11370.90660.94770.135*
H22B0.25480.86871.01970.135*
H22C0.12860.78951.05320.135*
C230.3709 (7)0.6488 (6)0.9891 (4)0.118 (2)
H23A0.41050.60490.94050.177*
H23B0.32340.59551.04960.177*
H23C0.45160.67251.01310.177*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.02636 (11)0.01654 (10)0.03726 (12)0.00540 (7)0.00062 (7)0.01261 (7)
O10.0260 (11)0.0386 (11)0.0424 (11)0.0067 (9)0.0057 (8)0.0140 (9)
O20.0319 (12)0.0424 (12)0.0433 (11)0.0115 (9)0.0017 (9)0.0139 (9)
O30.0467 (14)0.0443 (13)0.0622 (14)0.0143 (11)0.0238 (11)0.0283 (11)
O40.0743 (19)0.0414 (14)0.0691 (16)0.0119 (13)0.0278 (13)0.0256 (12)
O50.071 (2)0.0525 (16)0.101 (2)0.0199 (14)0.0489 (16)0.0380 (14)
O60.0440 (14)0.0504 (14)0.0415 (12)0.0020 (11)0.0028 (10)0.0107 (10)
O70.053 (2)0.0577 (19)0.136 (3)0.0091 (15)0.0075 (18)0.0079 (17)
O80.117 (3)0.103 (3)0.207 (5)0.016 (3)0.031 (3)0.094 (3)
O90.0556 (19)0.0490 (17)0.140 (3)0.0094 (14)0.0235 (17)0.0346 (17)
O1W0.0314 (12)0.0417 (13)0.0651 (14)0.0108 (10)0.0036 (10)0.0068 (10)
N10.0271 (13)0.0192 (11)0.0485 (13)0.0045 (9)0.0000 (10)0.0154 (9)
N20.0354 (14)0.0206 (11)0.0442 (13)0.0074 (10)0.0013 (10)0.0176 (9)
N30.067 (2)0.085 (2)0.0376 (16)0.0242 (19)0.0111 (14)0.0075 (15)
N40.048 (2)0.0435 (18)0.082 (2)0.0156 (15)0.0143 (16)0.0162 (16)
C10.0261 (15)0.0209 (13)0.0382 (14)0.0021 (10)0.0038 (11)0.0136 (10)
C20.0413 (19)0.0419 (18)0.0391 (16)0.0022 (14)0.0030 (13)0.0133 (13)
C30.045 (2)0.0462 (19)0.0393 (16)0.0087 (15)0.0126 (13)0.0168 (13)
C40.0386 (18)0.0471 (19)0.0437 (16)0.0108 (14)0.0100 (13)0.0241 (14)
C50.046 (2)0.0458 (19)0.0416 (16)0.0171 (15)0.0112 (13)0.0201 (14)
C60.0432 (19)0.0402 (17)0.0424 (16)0.0103 (14)0.0013 (13)0.0165 (13)
C70.0402 (19)0.0414 (18)0.0432 (16)0.0053 (14)0.0039 (13)0.0178 (13)
C80.043 (2)0.048 (2)0.064 (2)0.0125 (16)0.0207 (16)0.0238 (16)
C90.053 (2)0.0385 (18)0.064 (2)0.0141 (16)0.0206 (16)0.0226 (15)
C100.052 (2)0.044 (2)0.0466 (18)0.0062 (16)0.0070 (15)0.0173 (14)
C110.0347 (16)0.0250 (14)0.0473 (16)0.0079 (12)0.0073 (12)0.0198 (12)
C120.0342 (16)0.0243 (14)0.0431 (15)0.0092 (12)0.0067 (12)0.0146 (11)
C130.0296 (15)0.0186 (13)0.0395 (14)0.0058 (10)0.0031 (11)0.0135 (10)
C140.0381 (17)0.0232 (14)0.0516 (17)0.0076 (12)0.0113 (13)0.0192 (12)
C150.0321 (16)0.0223 (14)0.0550 (17)0.0101 (12)0.0089 (13)0.0142 (12)
C160.0368 (17)0.0273 (15)0.0560 (18)0.0141 (13)0.0092 (13)0.0212 (13)
C170.0345 (17)0.0276 (15)0.0587 (18)0.0085 (12)0.0114 (13)0.0247 (13)
C180.0285 (15)0.0208 (13)0.0392 (14)0.0050 (10)0.0014 (11)0.0161 (11)
C190.0383 (18)0.0313 (16)0.069 (2)0.0170 (13)0.0179 (15)0.0288 (14)
C200.0414 (19)0.0325 (16)0.072 (2)0.0119 (14)0.0160 (15)0.0332 (15)
C210.045 (2)0.052 (2)0.0461 (18)0.0156 (16)0.0003 (15)0.0119 (15)
C220.113 (4)0.113 (4)0.062 (3)0.055 (3)0.011 (3)0.037 (3)
C230.119 (5)0.124 (5)0.078 (3)0.006 (4)0.051 (3)0.007 (3)
Geometric parameters (Å, º) top
Cd1—O12.4304 (19)C4—C91.380 (4)
Cd1—O1i2.398 (2)C4—C51.386 (4)
Cd1—O22.5080 (19)C5—C61.378 (4)
Cd1—O62.381 (2)C5—H5A0.9300
Cd1—O1W2.370 (2)C6—C71.388 (4)
Cd1—N12.305 (2)C6—H60.9300
Cd1—N2ii2.294 (2)C7—C81.376 (4)
O1—C11.259 (3)C7—C101.482 (4)
O1—Cd1i2.3985 (19)C8—C91.387 (4)
O2—C11.251 (3)C8—H80.9300
O3—C41.363 (4)C9—H90.9300
O3—C31.436 (4)C11—C121.384 (3)
O4—C101.235 (4)C11—H11A0.9300
O5—C101.293 (4)C12—C131.387 (4)
O5—H50.8400C12—H12A0.9300
O6—C211.225 (4)C13—C141.394 (4)
O7—N41.245 (4)C13—C181.490 (3)
O8—N41.206 (4)C14—C151.376 (4)
O9—N41.218 (4)C14—H140.9300
O1W—H110.8400C15—H150.9300
O1W—H120.8400C16—C171.382 (4)
N1—C111.335 (4)C16—H160.9300
N1—C151.338 (3)C17—C181.385 (4)
N2—C201.332 (4)C17—H170.9300
N2—C161.333 (4)C18—C191.389 (4)
N2—Cd1iii2.294 (2)C19—C201.379 (4)
N3—C211.324 (4)C19—H190.9300
N3—C221.428 (5)C20—H200.9300
N3—C231.453 (6)C21—H210.9300
C1—C21.510 (4)C22—H22A0.9600
C2—C31.515 (4)C22—H22B0.9600
C2—H2A0.9700C22—H22C0.9600
C2—H2B0.9700C23—H23A0.9600
C3—H3A0.9700C23—H23B0.9600
C3—H3B0.9700C23—H23C0.9600
N2ii—Cd1—N1177.79 (8)C6—C5—H5A120.0
N2ii—Cd1—O1W92.00 (8)C4—C5—H5A120.0
N1—Cd1—O1W88.38 (8)C5—C6—C7120.4 (3)
N2ii—Cd1—O687.14 (8)C5—C6—H6119.8
N1—Cd1—O690.79 (8)C7—C6—H6119.8
O1W—Cd1—O679.50 (8)C8—C7—C6119.0 (3)
N2ii—Cd1—O1i91.36 (8)C8—C7—C10121.4 (3)
N1—Cd1—O1i87.59 (7)C6—C7—C10119.7 (3)
O1W—Cd1—O1i161.18 (7)C7—C8—C9121.2 (3)
O6—Cd1—O1i82.19 (7)C7—C8—H8119.4
N2ii—Cd1—O196.38 (7)C9—C8—H8119.4
N1—Cd1—O185.10 (7)C4—C9—C8119.2 (3)
O1W—Cd1—O1127.31 (7)C4—C9—H9120.4
O6—Cd1—O1152.60 (8)C8—C9—H9120.4
O1i—Cd1—O170.59 (7)O4—C10—O5123.4 (3)
N2ii—Cd1—O287.11 (7)O4—C10—C7121.0 (3)
N1—Cd1—O295.10 (7)O5—C10—C7115.6 (3)
O1W—Cd1—O276.40 (7)N1—C11—C12123.3 (3)
O6—Cd1—O2154.98 (8)N1—C11—H11A118.4
O1i—Cd1—O2122.27 (6)C12—C11—H11A118.4
O1—Cd1—O252.37 (6)C11—C12—C13119.5 (3)
C1—O1—Cd1i153.61 (18)C11—C12—H12A120.3
C1—O1—Cd195.24 (16)C13—C12—H12A120.3
Cd1i—O1—Cd1109.41 (7)C12—C13—C14117.1 (2)
C1—O2—Cd191.80 (16)C12—C13—C18121.2 (2)
C4—O3—C3117.4 (2)C14—C13—C18121.7 (2)
C10—O5—H5120.0C15—C14—C13119.6 (3)
C21—O6—Cd1117.7 (2)C15—C14—H14120.2
Cd1—O1W—H11109.5C13—C14—H14120.2
Cd1—O1W—H12109.5N1—C15—C14123.3 (3)
H11—O1W—H12109.5N1—C15—H15118.4
C11—N1—C15117.2 (2)C14—C15—H15118.4
C11—N1—Cd1121.05 (17)N2—C16—C17123.2 (3)
C15—N1—Cd1121.72 (18)N2—C16—H16118.4
C20—N2—C16117.1 (2)C17—C16—H16118.4
C20—N2—Cd1iii120.16 (18)C16—C17—C18119.8 (3)
C16—N2—Cd1iii122.71 (18)C16—C17—H17120.1
C21—N3—C22121.9 (4)C18—C17—H17120.1
C21—N3—C23119.2 (4)C17—C18—C19116.8 (2)
C22—N3—C23119.0 (4)C17—C18—C13122.0 (2)
O8—N4—O9120.3 (4)C19—C18—C13121.2 (2)
O8—N4—O7119.6 (4)C20—C19—C18119.7 (3)
O9—N4—O7120.1 (4)C20—C19—H19120.2
O2—C1—O1120.6 (2)C18—C19—H19120.2
O2—C1—C2120.1 (2)N2—C20—C19123.4 (3)
O1—C1—C2119.3 (2)N2—C20—H20118.3
C1—C2—C3113.3 (3)C19—C20—H20118.3
C1—C2—H2A108.9O6—C21—N3125.3 (4)
C3—C2—H2A108.9O6—C21—H21117.4
C1—C2—H2B108.9N3—C21—H21117.4
C3—C2—H2B108.9N3—C22—H22A109.5
H2A—C2—H2B107.7N3—C22—H22B109.5
O3—C3—C2106.8 (2)H22A—C22—H22B109.5
O3—C3—H3A110.4N3—C22—H22C109.5
C2—C3—H3A110.4H22A—C22—H22C109.5
O3—C3—H3B110.4H22B—C22—H22C109.5
C2—C3—H3B110.4N3—C23—H23A109.5
H3A—C3—H3B108.6N3—C23—H23B109.5
O3—C4—C9124.3 (3)H23A—C23—H23B109.5
O3—C4—C5115.8 (3)N3—C23—H23C109.5
C9—C4—C5120.0 (3)H23A—C23—H23C109.5
C6—C5—C4120.1 (3)H23B—C23—H23C109.5
N2ii—Cd1—O1—C181.21 (16)C3—O3—C4—C92.8 (5)
N1—Cd1—O1—C1100.43 (16)C3—O3—C4—C5176.5 (3)
O1W—Cd1—O1—C116.23 (19)O3—C4—C5—C6176.5 (3)
O6—Cd1—O1—C1177.34 (16)C9—C4—C5—C62.8 (5)
O1i—Cd1—O1—C1170.41 (19)C4—C5—C6—C70.1 (5)
O2—Cd1—O1—C10.14 (14)C5—C6—C7—C82.3 (5)
N2ii—Cd1—O1—Cd1i89.19 (9)C5—C6—C7—C10175.3 (3)
N1—Cd1—O1—Cd1i89.16 (9)C6—C7—C8—C91.7 (5)
O1W—Cd1—O1—Cd1i173.37 (7)C10—C7—C8—C9175.9 (3)
O6—Cd1—O1—Cd1i6.93 (19)O3—C4—C9—C8175.8 (3)
O1i—Cd1—O1—Cd1i0.0C5—C4—C9—C83.4 (5)
O2—Cd1—O1—Cd1i170.55 (12)C7—C8—C9—C41.2 (6)
N2ii—Cd1—O2—C1100.20 (16)C8—C7—C10—O4179.8 (3)
N1—Cd1—O2—C179.95 (16)C6—C7—C10—O42.6 (5)
O1W—Cd1—O2—C1167.04 (16)C8—C7—C10—O51.0 (5)
O6—Cd1—O2—C1177.12 (17)C6—C7—C10—O5176.6 (3)
O1i—Cd1—O2—C110.41 (17)C15—N1—C11—C120.7 (4)
O1—Cd1—O2—C10.14 (14)Cd1—N1—C11—C12179.3 (2)
N2ii—Cd1—O6—C21125.3 (2)N1—C11—C12—C130.3 (4)
N1—Cd1—O6—C2155.5 (2)C11—C12—C13—C141.4 (4)
O1W—Cd1—O6—C2132.7 (2)C11—C12—C13—C18177.1 (3)
O1i—Cd1—O6—C21142.9 (2)C12—C13—C14—C151.5 (4)
O1—Cd1—O6—C21136.3 (2)C18—C13—C14—C15177.0 (3)
O2—Cd1—O6—C2148.4 (3)C11—N1—C15—C140.6 (4)
O1W—Cd1—N1—C11119.7 (2)Cd1—N1—C15—C14179.2 (2)
O6—Cd1—N1—C1140.2 (2)C13—C14—C15—N10.5 (5)
O1i—Cd1—N1—C1141.9 (2)C20—N2—C16—C171.1 (5)
O1—Cd1—N1—C11112.6 (2)Cd1iii—N2—C16—C17176.5 (2)
O2—Cd1—N1—C11164.1 (2)N2—C16—C17—C180.3 (5)
O1W—Cd1—N1—C1561.8 (2)C16—C17—C18—C190.3 (4)
O6—Cd1—N1—C15141.2 (2)C16—C17—C18—C13179.7 (3)
O1i—Cd1—N1—C15136.6 (2)C12—C13—C18—C1717.2 (4)
O1—Cd1—N1—C1565.9 (2)C14—C13—C18—C17164.4 (3)
O2—Cd1—N1—C1514.4 (2)C12—C13—C18—C19162.9 (3)
Cd1—O2—C1—O10.3 (2)C14—C13—C18—C1915.6 (4)
Cd1—O2—C1—C2178.9 (2)C17—C18—C19—C200.0 (5)
Cd1i—O1—C1—O2159.6 (3)C13—C18—C19—C20180.0 (3)
Cd1—O1—C1—O20.3 (3)C16—N2—C20—C191.4 (5)
Cd1i—O1—C1—C219.6 (5)Cd1iii—N2—C20—C19176.2 (3)
Cd1—O1—C1—C2178.9 (2)C18—C19—C20—N20.9 (5)
O2—C1—C2—C333.5 (4)Cd1—O6—C21—N3156.6 (3)
O1—C1—C2—C3147.4 (3)C22—N3—C21—O61.3 (6)
C4—O3—C3—C2174.9 (3)C23—N3—C21—O6179.9 (4)
C1—C2—C3—O363.2 (3)
Symmetry codes: (i) x, y+2, z+1; (ii) x, y+1, z; (iii) x, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5···O4iv0.841.802.629 (3)171
O1W—H11···O70.841.942.754 (4)164
O1W—H12···O2v0.842.032.763 (3)145
Symmetry codes: (iv) x+2, y+1, z; (v) x+1, y+2, z+1.

Experimental details

Crystal data
Chemical formula[Cd2(C10H9O5)2(C10H8N2)2(C3H7NO)2(H2O)2](NO3)2
Mr1261.76
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)9.1020 (5), 11.6866 (5), 13.3534 (5)
α, β, γ (°)69.1646 (11), 84.2052 (16), 76.9358 (16)
V3)1292.84 (10)
Z1
Radiation typeMo Kα
µ (mm1)0.91
Crystal size (mm)0.19 × 0.12 × 0.11
Data collection
DiffractometerRigaku R-AXIS RAPID IP
diffractometer
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.847, 0.907
No. of measured, independent and
observed [I > 2σ(I)] reflections
12594, 5822, 4760
Rint0.031
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.077, 1.08
No. of reflections5822
No. of parameters345
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.95, 0.59

Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalClear (Rigaku, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5···O4i0.841.802.629 (3)171
O1W—H11···O70.841.942.754 (4)164
O1W—H12···O2ii0.842.032.763 (3)145
Symmetry codes: (i) x+2, y+1, z; (ii) x+1, y+2, z+1.
 

Acknowledgements

This work is supported by the Key Project of the Natural Science Foundation of Heilongjiang Province (grant No. ZD200903), the Key Project of the Education Bureau of Heilongjiang Province (grants No. 12511z023, No. 2011CJHB006), the Innovation Team of the Education Bureau of Heilongjiang Province (grant No. 2010 t d03), Heilongjiang University (Hdtd2010–04) and the Ministry of Higher Education of Malaysia (grant No. UM.C/HIR/MOHE/SC/12).

References

First citationBarbour, L. J. (2001). J. Supramol. Chem. 1, 189–191.  CrossRef CAS Google Scholar
First citationGao, S. & Ng, S. W. (2006). Acta Cryst. E62, o3420–o3421.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationHigashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.  Google Scholar
First citationRigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.  Google Scholar
First citationRigaku (2002). CrystalClear. Rigaku/MSC Inc., The Woodlands, Texas, USA.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationWestrip, S. P. (2010). J. Appl. Cryst. 43, 920–925.  Web of Science CrossRef CAS IUCr Journals Google Scholar

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.

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds