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Acta Cryst. (2007). E63, m2889    [ doi:10.1107/S1600536807051665 ]

Poly[[tris(1,10-phenanthroline)tris([mu]3-succinato)tricadmium(II)] tetrahydrate]

X.-Y. Wang, X.-T. Deng, C.-G. Wang and M. Wang

Abstract top

The title complex, {[Cd3(C4H4O4)3(C12H8N2)3]·4H2O}n, has been isolated from the hydrothermal reaction of cadmium acetate with 1,10-phenanthroline (phen) and succinic acid. The structure features two-dimensional networks formed by succinate ligands bridging Cd atoms in two different coordination modes. A twofold rotation axis passes through one Cd atom. In one coordination mode, the Cd atoms are in a distorted octahedral CdO4N2 arrangement and the coordination atoms come from one phen ligand and two succinate ligands. In the other coordination mode, the Cd atoms are in the decahedral CdO5N2 geometries and the coordination atoms come from one phen ligand and three succinate ligands.

Comment top

Succinic acid is a flexible bridging spacer to constitute coordination polymers. The simultaneous coordination of hydroxide and succinate groups to transition metal atoms tends to form coordination polymers with three-dimensional open framework [Zheng et al. (2001)] . Introduction of a second competing ligand such as phen has been found to lower the dimensionality of the structure since its chelation to the metal ion leaves fewer sites for succinate coordination. In structure (I), the Cd atoms are in the distorted octahedral CdO4N2 and decahedral CdO5N2 geometries. (Fig. 1) The succinato ligands have two coordination modes (Fig. 2). In the first mode, the carboxylate group bidentately bridges two Cd atoms. In the other mode, one chelating O atom bonds to the second Cd atom. The Cd atoms are interlinked by the succinate ligands to generate two-dimensional networks, in which existing stacking interactions between phen rings and hydrogen bonds.

Related literature top

For related literature, see: Zheng & Lin (2001).

Experimental top

A mixture of Cd(CH3COO)2˙2H2O (0.266 g, 1 mmol), succinic acid (0.465 g, 4 mmol), 1,10-phenanthroline hydrate (0.396 g, 2 mmol) and H2O (10 ml) was heated in a 23 ml stainless steel reactor with a Teflon liner at 453 K for 72 h. Colorless block-shape crystals of the title complex were obtained.

Refinement top

H atoms bonded to O atoms were located in difference maps and then included in the refinement with bond-length restraints of O–H = 0.82 (2) Å, with Uiso(H)= 1.5Ueq All other H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms with C–H distances of 0.93 and 0.97 Å and Uiso(H) = 1.2Ueq(C) or 1.5Ueq.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SMART (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: SHELXTL (Bruker, 1997).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), with displacement ellipsoids drawn at the 50% probability level. The H atoms and water molecules have been omitted for clarity. [symmety codes:(a) −x,y, 1/2 − z;(b) 1 − x,y, 1/2 − z; (d) −x,-y,1 − z]
[Figure 2] Fig. 2. The molecular structure of (I), showing two-dimensional networks omitting water molecules and phen ligands.
Poly[[[(1,10-phenanthroline)cadmium(II)]-µ-succnicate-κ4O,O,O'O'] hydrate] top
Crystal data top
[Cd3(C4H4O4)3(C12H8N2)3]·4H2OF000 = 2584
Mr = 1298.09Dx = 1.811 Mg m−3
Monoclinic, C2/cMo Kα radiation
λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 6336 reflections
a = 11.1875 (6) Åθ = 2.5–28.2º
b = 21.4051 (15) ŵ = 1.41 mm−1
c = 20.2455 (12) ÅT = 298 (2) K
β = 100.8470 (10)ºBlock, colorless
V = 4761.6 (5) Å30.32 × 0.20 × 0.20 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer		5526 independent reflections
Radiation source: fine-focus sealed tube4640 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.073
T = 298(2) Kθmax = 27.8º
φ and ω scansθmin = 1.9º
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −14→14
Tmin = 0.662, Tmax = 0.766k = −22→27
16149 measured reflectionsl = −18→26
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.035H atoms treated by a mixture of
independent and constrained refinement
wR(F2) = 0.073  w = 1/[σ2(Fo2) + (0.0314P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.97(Δ/σ)max = 0.002
5526 reflectionsΔρmax = 0.74 e Å−3
343 parametersΔρmin = −0.78 e Å−3
4 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00223 (7)
Crystal data top
[Cd3(C4H4O4)3(C12H8N2)3]·4H2OV = 4761.6 (5) Å3
Mr = 1298.09Z = 4
Monoclinic, C2/cMo Kα
a = 11.1875 (6) ŵ = 1.41 mm−1
b = 21.4051 (15) ÅT = 298 (2) K
c = 20.2455 (12) Å0.32 × 0.20 × 0.20 mm
β = 100.8470 (10)º
Data collection top
Bruker SMART CCD area-detector
diffractometer		5526 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		4640 reflections with I > 2σ(I)
Tmin = 0.662, Tmax = 0.766Rint = 0.073
16149 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0354 restraints
wR(F2) = 0.073H atoms treated by a mixture of
independent and constrained refinement
S = 0.97Δρmax = 0.74 e Å−3
5526 reflectionsΔρmin = −0.78 e Å−3
343 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*/Ueq
Cd10.50000.450298 (13)0.25000.03689 (9)
Cd20.785266 (16)0.558555 (9)0.372822 (9)0.02702 (8)
N10.4185 (2)0.36355 (11)0.18944 (13)0.0408 (6)
N20.73872 (19)0.66078 (10)0.33202 (11)0.0320 (5)
N30.86461 (19)0.63215 (11)0.45773 (11)0.0324 (5)
O10.63997 (18)0.46118 (10)0.18172 (10)0.0470 (5)
O20.66807 (15)0.51931 (9)0.27212 (9)0.0328 (4)
O31.0882 (2)0.46530 (13)0.15096 (13)0.0661 (7)
O41.01226 (19)0.56006 (11)0.14051 (11)0.0531 (6)
O50.59517 (19)0.55649 (11)0.41393 (12)0.0566 (7)
O60.74168 (19)0.49423 (10)0.45879 (11)0.0498 (5)
C10.7021 (2)0.50054 (12)0.21886 (13)0.0296 (6)
C20.8143 (2)0.52649 (13)0.19883 (13)0.0321 (6)
H2A0.86720.54320.23840.038*
H2B0.79140.56070.16760.038*
C30.8840 (2)0.47844 (15)0.16635 (17)0.0467 (8)
H3A0.90040.44260.19600.056*
H3B0.83320.46440.12480.056*
C41.0029 (3)0.50216 (17)0.15113 (14)0.0446 (8)
C50.3448 (3)0.36281 (16)0.13045 (17)0.0515 (8)
H50.31450.40070.11210.062*
C60.3099 (3)0.30888 (18)0.09421 (18)0.0598 (9)
H60.25960.31080.05210.072*
C70.3511 (3)0.25281 (17)0.12167 (18)0.0571 (9)
H70.32900.21600.09820.069*
C80.4264 (3)0.25086 (14)0.18520 (16)0.0423 (7)
C90.4599 (2)0.30787 (13)0.21748 (14)0.0362 (6)
C100.4661 (3)0.19347 (15)0.21870 (16)0.0549 (9)
H100.44490.15570.19700.066*
C110.6760 (3)0.67523 (14)0.27157 (14)0.0408 (7)
H110.64290.64300.24310.049*
C120.6576 (3)0.73636 (16)0.24886 (15)0.0491 (8)
H120.61250.74450.20630.059*
C130.7060 (3)0.78405 (14)0.28923 (16)0.0468 (8)
H130.69560.82510.27410.056*
C140.7718 (2)0.77134 (13)0.35386 (14)0.0367 (6)
C150.8255 (3)0.81935 (14)0.39966 (17)0.0464 (7)
H150.81720.86100.38640.056*
C160.8867 (3)0.80530 (15)0.46072 (16)0.0491 (8)
H160.91980.83730.48950.059*
C170.9027 (2)0.74159 (14)0.48317 (14)0.0388 (7)
C180.9684 (3)0.72468 (15)0.54706 (15)0.0475 (8)
H181.00300.75520.57740.057*
C190.9806 (3)0.66304 (16)0.56400 (15)0.0483 (8)
H191.02380.65110.60590.058*
C200.9279 (3)0.61835 (14)0.51804 (14)0.0402 (7)
H200.93750.57650.53020.048*
C210.8526 (2)0.69322 (13)0.43960 (12)0.0308 (6)
C220.7853 (2)0.70819 (13)0.37350 (13)0.0310 (6)
C230.6369 (3)0.51558 (15)0.45537 (15)0.0413 (7)
C240.5619 (3)0.48871 (19)0.50365 (18)0.0600 (10)
H24A0.55930.44370.49830.072*
H24B0.60370.49750.54920.072*
O70.3967 (2)0.64187 (12)0.38792 (14)0.0622 (7)
H7A0.345 (3)0.630 (2)0.407 (2)0.093*
H7B0.449 (3)0.6154 (16)0.393 (2)0.093*
O80.8093 (2)0.39279 (12)0.54661 (12)0.0548 (6)
H8A0.870 (2)0.4015 (19)0.5751 (16)0.082*
H8B0.795 (4)0.4228 (14)0.5223 (18)0.082*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.02758 (14)0.02503 (16)0.0631 (2)0.0000.02148 (13)0.000
Cd20.02656 (11)0.02609 (12)0.03117 (12)−0.00091 (7)0.01250 (8)−0.00017 (8)
N10.0353 (12)0.0292 (13)0.0587 (16)−0.0019 (10)0.0106 (11)0.0041 (11)
N20.0343 (11)0.0322 (13)0.0310 (12)0.0016 (10)0.0103 (9)0.0010 (10)
N30.0362 (12)0.0311 (13)0.0324 (12)0.0007 (9)0.0128 (10)0.0015 (10)
O10.0385 (11)0.0575 (14)0.0496 (13)−0.0221 (10)0.0201 (10)−0.0225 (11)
O20.0295 (9)0.0364 (11)0.0350 (10)−0.0037 (8)0.0127 (8)−0.0059 (8)
O30.0409 (12)0.0809 (19)0.0837 (18)−0.0104 (12)0.0299 (12)−0.0349 (15)
O40.0417 (12)0.0665 (17)0.0543 (14)−0.0193 (11)0.0172 (10)0.0069 (12)
O50.0424 (12)0.0763 (18)0.0572 (14)0.0027 (11)0.0247 (11)0.0284 (12)
O60.0500 (12)0.0432 (13)0.0642 (14)0.0047 (10)0.0316 (11)0.0120 (11)
C10.0264 (12)0.0305 (15)0.0335 (14)0.0007 (10)0.0101 (11)0.0031 (11)
C20.0320 (13)0.0345 (15)0.0319 (14)−0.0093 (11)0.0116 (11)−0.0011 (11)
C30.0364 (15)0.0452 (19)0.064 (2)−0.0122 (13)0.0230 (15)−0.0141 (16)
C40.0331 (15)0.072 (2)0.0319 (16)−0.0175 (15)0.0157 (12)−0.0220 (15)
C50.0461 (18)0.046 (2)0.060 (2)−0.0029 (15)0.0047 (16)0.0103 (16)
C60.055 (2)0.065 (3)0.056 (2)−0.0097 (18)0.0013 (17)0.0028 (18)
C70.055 (2)0.050 (2)0.067 (2)−0.0192 (17)0.0125 (17)−0.0137 (18)
C80.0390 (15)0.0310 (16)0.061 (2)−0.0066 (12)0.0186 (15)−0.0038 (14)
C90.0298 (13)0.0275 (15)0.0547 (18)−0.0018 (11)0.0167 (12)−0.0005 (12)
C100.061 (2)0.0271 (16)0.080 (3)−0.0087 (14)0.0217 (18)−0.0086 (15)
C110.0446 (16)0.0415 (18)0.0365 (16)0.0027 (13)0.0082 (13)−0.0006 (13)
C120.0499 (18)0.058 (2)0.0382 (17)0.0103 (16)0.0056 (14)0.0115 (15)
C130.0520 (18)0.0348 (17)0.057 (2)0.0097 (14)0.0190 (16)0.0129 (15)
C140.0374 (14)0.0297 (15)0.0468 (17)0.0027 (12)0.0172 (13)0.0032 (12)
C150.0513 (18)0.0258 (16)0.063 (2)−0.0011 (13)0.0137 (16)−0.0008 (14)
C160.0548 (18)0.0301 (17)0.061 (2)−0.0092 (14)0.0079 (16)−0.0080 (15)
C170.0391 (15)0.0344 (16)0.0444 (17)−0.0051 (12)0.0118 (13)−0.0064 (13)
C180.0512 (18)0.048 (2)0.0405 (18)−0.0096 (15)0.0005 (14)−0.0127 (15)
C190.0488 (18)0.058 (2)0.0365 (17)−0.0036 (16)0.0026 (14)0.0002 (15)
C200.0440 (16)0.0386 (17)0.0385 (16)0.0026 (13)0.0090 (13)0.0035 (13)
C210.0305 (13)0.0308 (15)0.0341 (15)−0.0005 (11)0.0138 (11)−0.0013 (11)
C220.0293 (13)0.0297 (15)0.0367 (15)−0.0010 (11)0.0129 (11)−0.0001 (12)
C230.0432 (16)0.0452 (18)0.0407 (17)−0.0085 (14)0.0210 (13)0.0028 (14)
C240.0496 (19)0.076 (3)0.062 (2)0.0037 (18)0.0282 (17)0.0248 (19)
O70.0657 (17)0.0497 (16)0.0671 (17)−0.0044 (13)0.0022 (13)0.0110 (13)
O80.0580 (14)0.0522 (15)0.0531 (16)0.0038 (12)0.0081 (11)0.0067 (11)
Geometric parameters (Å, °) top
Cd1—O1i2.2873 (19)C6—C71.366 (5)
Cd1—O12.2873 (19)C6—H60.9300
Cd1—N12.315 (2)C7—C81.399 (4)
Cd1—N1i2.315 (2)C7—H70.9300
Cd1—O22.3667 (17)C8—C91.402 (4)
Cd1—O2i2.3667 (17)C8—C101.433 (4)
Cd1—C1i2.683 (2)C9—C9i1.447 (5)
Cd2—O4ii2.331 (2)C10—C10i1.349 (6)
Cd2—O62.341 (2)C10—H100.9300
Cd2—O22.3613 (17)C11—C121.389 (4)
Cd2—N22.362 (2)C11—H110.9300
Cd2—N32.377 (2)C12—C131.355 (4)
Cd2—O52.426 (2)C12—H120.9300
Cd2—O3ii2.545 (3)C13—C141.402 (4)
N1—C51.318 (4)C13—H130.9300
N1—C91.363 (3)C14—C221.409 (4)
N2—C111.328 (3)C14—C151.438 (4)
N2—C221.357 (3)C15—C161.330 (4)
N3—C201.324 (3)C15—H150.9300
N3—C211.357 (4)C16—C171.438 (4)
O1—C11.249 (3)C16—H160.9300
O2—C11.274 (3)C17—C211.407 (4)
O3—C41.239 (4)C17—C181.409 (4)
O3—Cd2ii2.545 (3)C18—C191.364 (4)
O4—C41.265 (4)C18—H180.9300
O4—Cd2ii2.331 (2)C19—C201.386 (4)
O5—C231.241 (4)C19—H190.9300
O6—C231.248 (3)C20—H200.9300
C1—C21.497 (3)C21—C221.443 (3)
C2—C31.514 (4)C23—C241.516 (4)
C2—H2A0.9700C24—C24iii1.448 (6)
C2—H2B0.9700C24—H24A0.9700
C3—C41.509 (4)C24—H24B0.9700
C3—H3A0.9700O7—H7A0.791 (18)
C3—H3B0.9700O7—H7B0.804 (18)
C5—C61.384 (5)O8—H8A0.823 (18)
C5—H50.9300O8—H8B0.806 (19)
O1i—Cd1—O1168.31 (11)C4—C3—H3B108.8
O1i—Cd1—N198.96 (9)C2—C3—H3B108.8
O1—Cd1—N190.44 (8)H3A—C3—H3B107.7
O1i—Cd1—N1i90.44 (8)O3—C4—O4122.3 (3)
O1—Cd1—N1i98.96 (9)O3—C4—C3119.7 (3)
N1—Cd1—N1i73.37 (12)O4—C4—C3117.9 (3)
O1i—Cd1—O2115.59 (7)N1—C5—C6123.8 (3)
O1—Cd1—O256.00 (6)N1—C5—H5118.1
N1—Cd1—O2145.11 (7)C6—C5—H5118.1
N1i—Cd1—O2100.42 (7)C7—C6—C5118.5 (3)
O1i—Cd1—O2i56.00 (6)C7—C6—H6120.7
O1—Cd1—O2i115.59 (7)C5—C6—H6120.7
N1—Cd1—O2i100.42 (7)C6—C7—C8119.9 (3)
N1i—Cd1—O2i145.11 (7)C6—C7—H7120.0
O2—Cd1—O2i102.76 (9)C8—C7—H7120.0
O1i—Cd1—C1i27.67 (7)C7—C8—C9117.7 (3)
O1—Cd1—C1i143.51 (8)C7—C8—C10122.7 (3)
N1—Cd1—C1i100.42 (8)C9—C8—C10119.6 (3)
N1i—Cd1—C1i117.52 (8)N1—C9—C8121.8 (3)
O2—Cd1—C1i112.32 (7)N1—C9—C9i118.86 (16)
O2i—Cd1—C1i28.34 (7)C8—C9—C9i119.32 (18)
O4ii—Cd2—O6115.91 (8)C10i—C10—C8120.94 (18)
O4ii—Cd2—O2107.38 (7)C10i—C10—H10119.5
O6—Cd2—O2105.85 (7)C8—C10—H10119.5
O4ii—Cd2—N295.84 (8)N2—C11—C12123.0 (3)
O6—Cd2—N2137.87 (7)N2—C11—H11118.5
O2—Cd2—N288.71 (7)C12—C11—H11118.5
O4ii—Cd2—N380.55 (7)C13—C12—C11119.5 (3)
O6—Cd2—N387.36 (8)C13—C12—H12120.3
O2—Cd2—N3158.64 (7)C11—C12—H12120.3
N2—Cd2—N370.53 (7)C12—C13—C14119.8 (3)
O4ii—Cd2—O5166.83 (8)C12—C13—H13120.1
O6—Cd2—O554.24 (7)C14—C13—H13120.1
O2—Cd2—O584.81 (7)C13—C14—C22117.3 (3)
N2—Cd2—O589.26 (7)C13—C14—C15123.1 (3)
N3—Cd2—O589.78 (8)C22—C14—C15119.6 (3)
O4ii—Cd2—O3ii53.26 (7)C16—C15—C14121.2 (3)
O6—Cd2—O3ii83.13 (7)C16—C15—H15119.4
O2—Cd2—O3ii78.21 (8)C14—C15—H15119.4
N2—Cd2—O3ii138.96 (7)C15—C16—C17121.3 (3)
N3—Cd2—O3ii120.76 (8)C15—C16—H16119.3
O5—Cd2—O3ii127.25 (8)C17—C16—H16119.3
C5—N1—C9118.2 (3)C21—C17—C18117.6 (3)
C5—N1—Cd1127.3 (2)C21—C17—C16119.2 (3)
C9—N1—Cd1114.31 (19)C18—C17—C16123.1 (3)
C11—N2—C22118.1 (2)C19—C18—C17119.3 (3)
C11—N2—Cd2125.57 (19)C19—C18—H18120.3
C22—N2—Cd2116.27 (17)C17—C18—H18120.3
C20—N3—C21118.2 (2)C18—C19—C20119.3 (3)
C20—N3—Cd2125.52 (19)C18—C19—H19120.4
C21—N3—Cd2115.99 (17)C20—C19—H19120.4
C1—O1—Cd194.09 (16)N3—C20—C19123.4 (3)
C1—O2—Cd2129.59 (15)N3—C20—H20118.3
C1—O2—Cd189.78 (15)C19—C20—H20118.3
Cd2—O2—Cd1132.66 (8)N3—C21—C17122.1 (2)
C4—O3—Cd2ii87.5 (2)N3—C21—C22118.2 (2)
C4—O4—Cd2ii96.86 (18)C17—C21—C22119.7 (3)
C23—O5—Cd290.14 (17)N2—C22—C14122.3 (2)
C23—O6—Cd293.92 (18)N2—C22—C21118.7 (2)
O1—C1—O2120.1 (2)C14—C22—C21119.0 (2)
O1—C1—C2119.1 (2)O5—C23—O6121.7 (3)
O2—C1—C2120.8 (2)O5—C23—C24121.3 (3)
C1—C2—C3113.1 (2)O6—C23—C24117.0 (3)
C1—C2—H2A109.0C24iii—C24—C23116.3 (4)
C3—C2—H2A109.0C24iii—C24—H24A108.2
C1—C2—H2B109.0C23—C24—H24A108.2
C3—C2—H2B109.0C24iii—C24—H24B108.2
H2A—C2—H2B107.8C23—C24—H24B108.2
C4—C3—C2114.0 (3)H24A—C24—H24B107.4
C4—C3—H3A108.8H7A—O7—H7B107 (4)
C2—C3—H3A108.8H8A—O8—H8B107 (4)
O1i—Cd1—N1—C595.2 (3)O5—Cd2—O6—C23−0.51 (18)
O1—Cd1—N1—C5−77.8 (3)O3ii—Cd2—O6—C23−147.46 (19)
N1i—Cd1—N1—C5−177.0 (3)Cd1—O1—C1—O2−2.2 (3)
O2—Cd1—N1—C5−92.7 (3)Cd1—O1—C1—C2179.6 (2)
O2i—Cd1—N1—C538.4 (3)Cd2—O2—C1—O1153.3 (2)
C1i—Cd1—N1—C567.2 (3)Cd1—O2—C1—O12.1 (3)
O1i—Cd1—N1—C9−89.39 (19)Cd2—O2—C1—C2−28.5 (3)
O1—Cd1—N1—C997.6 (2)Cd1—O2—C1—C2−179.7 (2)
N1i—Cd1—N1—C9−1.62 (14)O1—C1—C2—C3−37.5 (4)
O2—Cd1—N1—C982.7 (2)O2—C1—C2—C3144.2 (3)
O2i—Cd1—N1—C9−146.26 (19)C1—C2—C3—C4−175.1 (2)
C1i—Cd1—N1—C9−117.43 (19)Cd2ii—O3—C4—O40.8 (3)
O4ii—Cd2—N2—C11103.4 (2)Cd2ii—O3—C4—C3−177.5 (2)
O6—Cd2—N2—C11−116.4 (2)Cd2ii—O4—C4—O3−0.8 (3)
O2—Cd2—N2—C11−4.0 (2)Cd2ii—O4—C4—C3177.4 (2)
N3—Cd2—N2—C11−178.8 (2)C2—C3—C4—O3150.8 (3)
O5—Cd2—N2—C11−88.8 (2)C2—C3—C4—O4−27.5 (4)
O3ii—Cd2—N2—C1166.3 (3)C9—N1—C5—C6−2.2 (5)
O4ii—Cd2—N2—C22−73.61 (18)Cd1—N1—C5—C6173.0 (3)
O6—Cd2—N2—C2266.6 (2)N1—C5—C6—C72.0 (5)
O2—Cd2—N2—C22179.05 (18)C5—C6—C7—C80.2 (5)
N3—Cd2—N2—C224.20 (17)C6—C7—C8—C9−1.9 (5)
O5—Cd2—N2—C2294.23 (18)C6—C7—C8—C10175.8 (3)
O3ii—Cd2—N2—C22−110.64 (19)C5—N1—C9—C80.3 (4)
O4ii—Cd2—N3—C20−78.7 (2)Cd1—N1—C9—C8−175.6 (2)
O6—Cd2—N3—C2038.1 (2)C5—N1—C9—C9i−179.5 (3)
O2—Cd2—N3—C20167.36 (19)Cd1—N1—C9—C9i4.7 (4)
N2—Cd2—N3—C20−178.4 (2)C7—C8—C9—N11.7 (4)
O5—Cd2—N3—C2092.3 (2)C10—C8—C9—N1−176.0 (3)
O3ii—Cd2—N3—C20−42.3 (2)C7—C8—C9—C9i−178.5 (3)
O4ii—Cd2—N3—C2194.91 (18)C10—C8—C9—C9i3.7 (5)
O6—Cd2—N3—C21−148.27 (18)C7—C8—C10—C10i−176.7 (4)
O2—Cd2—N3—C21−19.0 (3)C9—C8—C10—C10i0.9 (6)
N2—Cd2—N3—C21−4.78 (17)C22—N2—C11—C120.9 (4)
O5—Cd2—N3—C21−94.07 (18)Cd2—N2—C11—C12−176.0 (2)
O3ii—Cd2—N3—C21131.33 (17)N2—C11—C12—C130.6 (5)
O1i—Cd1—O1—C147.76 (16)C11—C12—C13—C14−1.3 (5)
N1—Cd1—O1—C1−168.60 (18)C12—C13—C14—C220.6 (4)
N1i—Cd1—O1—C1−95.37 (18)C12—C13—C14—C15−179.8 (3)
O2—Cd1—O1—C11.21 (15)C13—C14—C15—C16179.7 (3)
O2i—Cd1—O1—C189.62 (17)C22—C14—C15—C16−0.8 (5)
C1i—Cd1—O1—C183.1 (2)C14—C15—C16—C170.6 (5)
O4ii—Cd2—O2—C11.1 (2)C15—C16—C17—C210.0 (5)
O6—Cd2—O2—C1−123.3 (2)C15—C16—C17—C18179.1 (3)
N2—Cd2—O2—C196.8 (2)C21—C17—C18—C190.0 (4)
N3—Cd2—O2—C1110.3 (3)C16—C17—C18—C19−179.1 (3)
O5—Cd2—O2—C1−173.8 (2)C17—C18—C19—C20−0.2 (5)
O3ii—Cd2—O2—C1−44.0 (2)C21—N3—C20—C191.2 (4)
O4ii—Cd2—O2—Cd1140.17 (11)Cd2—N3—C20—C19174.7 (2)
O6—Cd2—O2—Cd115.78 (12)C18—C19—C20—N3−0.4 (5)
N2—Cd2—O2—Cd1−124.11 (11)C20—N3—C21—C17−1.4 (4)
N3—Cd2—O2—Cd1−110.69 (18)Cd2—N3—C21—C17−175.53 (19)
O5—Cd2—O2—Cd1−34.73 (11)C20—N3—C21—C22179.1 (2)
O3ii—Cd2—O2—Cd195.05 (12)Cd2—N3—C21—C225.0 (3)
O1i—Cd1—O2—C1−171.79 (14)C18—C17—C21—N30.9 (4)
O1—Cd1—O2—C1−1.18 (15)C16—C17—C21—N3180.0 (3)
N1—Cd1—O2—C116.8 (2)C18—C17—C21—C22−179.6 (2)
N1i—Cd1—O2—C192.65 (15)C16—C17—C21—C22−0.5 (4)
O2i—Cd1—O2—C1−113.61 (15)C11—N2—C22—C14−1.6 (4)
C1i—Cd1—O2—C1−141.66 (14)Cd2—N2—C22—C14175.58 (19)
O1i—Cd1—O2—Cd238.54 (13)C11—N2—C22—C21179.4 (2)
O1—Cd1—O2—Cd2−150.85 (14)Cd2—N2—C22—C21−3.4 (3)
N1—Cd1—O2—Cd2−132.82 (13)C13—C14—C22—N20.9 (4)
N1i—Cd1—O2—Cd2−57.02 (12)C15—C14—C22—N2−178.7 (2)
O2i—Cd1—O2—Cd296.72 (11)C13—C14—C22—C21179.8 (2)
C1i—Cd1—O2—Cd268.67 (12)C15—C14—C22—C210.2 (4)
O4ii—Cd2—O5—C23−43.9 (5)N3—C21—C22—N2−1.1 (3)
O6—Cd2—O5—C230.51 (18)C17—C21—C22—N2179.4 (2)
O2—Cd2—O5—C23114.3 (2)N3—C21—C22—C14179.9 (2)
N2—Cd2—O5—C23−156.9 (2)C17—C21—C22—C140.4 (4)
N3—Cd2—O5—C23−86.4 (2)Cd2—O5—C23—O6−0.9 (3)
O3ii—Cd2—O5—C2343.4 (2)Cd2—O5—C23—C24179.8 (3)
O4ii—Cd2—O6—C23169.29 (18)Cd2—O6—C23—O50.9 (3)
O2—Cd2—O6—C23−71.82 (19)Cd2—O6—C23—C24−179.8 (3)
N2—Cd2—O6—C2334.4 (2)O5—C23—C24—C24iii2.8 (6)
N3—Cd2—O6—C2391.13 (19)O6—C23—C24—C24iii−176.5 (4)
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) −x+2, y, −z+1/2; (iii) −x+1, −y+1, −z+1.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O7—H7A···O8iii0.791 (18)2.174 (19)2.962 (4)174 (5)
O7—H7B···O50.804 (18)2.048 (19)2.847 (3)172 (4)
O8—H8A···O4iv0.823 (18)2.04 (2)2.857 (3)169 (4)
O8—H8B···O60.806 (19)2.015 (19)2.818 (3)174 (4)
Symmetry codes: (iii) −x+1, −y+1, −z+1; (iv) x, −y+1, z+1/2.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O7—H7A···O8i0.791 (18)2.174 (19)2.962 (4)174 (5)
O7—H7B···O50.804 (18)2.048 (19)2.847 (3)172 (4)
O8—H8A···O4ii0.823 (18)2.04 (2)2.857 (3)169 (4)
O8—H8B···O60.806 (19)2.015 (19)2.818 (3)174 (4)
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, −y+1, z+1/2.
Acknowledgements top

This work was supported by the Hubei Key Laboratory of Novel Chemical Reactor and Green Chemical Technology (grant No. RCT2004011).

references
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