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Acta Cryst. (2007). E63, m2392    [ doi:10.1107/S1600536807040214 ]

catena-Poly[[[aqua(1,10-phenanthroline-[kappa]2N,N')cadmium(II)]-[mu]-o-phenylenediacetato-[kappa]2O,O':[kappa]O''-[bis(1,10-phenanthroline-[kappa]2N,N')cadmium(II)]-[mu]-o-phenylenediacetato-[kappa]O:[kappa]2O',O''] ethanol 0.79-solvate 3.05-hydrate]

Y. Yang, M.-H. Zeng, S.-H. Zhang and H. Liang

Abstract top

In the title compound, [Cd2(C10H8O4)2(C12H8N2)3(H2O)]·0.79C2H6O·3.05H2O, the two independent CdII atoms in the asymmetric unit have different coordination modes. One is six-coordinate and the other is seven-coordinate, forming distorted octahedral and monocapped octahedral geometries, respectively. The CdII atoms are bridged by o-phenylenediacetate ligands to form a one-dimensional chain structure, which is further linked into a two-dimensional network through O-H...O hydrogen bonds.

Comment top

Many complexes containing phenanthroline have been reported (e.g. Yam,et al.,1999; Harvey et al., 2000; Ding,et al.,2005) and these include dinuclear complexes containing phenanthroline bridged by carboxylate ligands (Tan, et al.,2006; Shi, et al.,2005). In this report we used phenanthroline, (2-Carboxymethyl-phenyl)-acetic acid and cadmium chloride to construct the title one-dimensional chain polymer.

The asymmetric unit contains two independent CdII atoms, two L2− ligands, three phenanthroline ligands, 3.05 H2O molecules and one partial occupancy C2H5OH molecule. The two CdII atoms have different coordination modes. Atom Cd1 is coordinated by four O atoms from two different L2− ligands, two N atoms from one phenanthroline ligand and by atom O9 from a water molecule, forming a distorted monocapped octahedral geometry. Atom Cd2 is coordinated by four N atoms from two different phenanthroline ligands and two O atoms from a two bridging L2−, ligands, forming a distorted octahedral geometry. The two independent CdII atoms are bridged by a L2− ligand forming a one-dimensional chain structure. Part of the one dimensional chain structure is shown in Fig. 1. A l l bond distances and angles are as expected. In the crystal structure, intermolecular O—H···O hydrogen bonds connect molecules to form a two-dimensional network (Fig. 2).

Related literature top

For related literature, see: Yam et al. (1999); Harvey et al. (2000); Ding et al. (2005); Shi et al. (2005); Tan et al. (2006).

Experimental top

A solution of (2-Carboxymethyl-phenyl)-acetic acid(2 mmol,0.388 g), phenanthroline(3 mmol,0.594 g),cadmium chloride(3 mmol,0.37 g) in the mixture solution of ethanol-water. The mixture solution was stirred for 30 min at room temperature,then filtered. The filtrate were added to 30 ml sealed teflon-lined stainless steel vessels, and the teflon-lined stainless steel vessels was placed at 413 K vacuum case for 4 d under autogenous pressure. After cooled to room temperature, colorless crystals were produced(yield: 48.8%, based on Cd).

Refinement top

The crystal contains various partial occupancy solvent molecules, namely a 0.79 occupancy ethanol molecule and in addition to the two full occupancy water solvent molecules there are two more sites for water atoms adding to a further occupancy of 1.05. The H atoms of the partial occupancy water atoms were not located and were not included in the refinement. The contribution of these H atoms is included in the molecular formula.

H atoms boned to C and N atoms were positioned geometrically and refined in a riding-model approximation, with C—H distances of 0.95–0.99 Å, N—H distances of 0.92 Å, and with Uiso(H) = 1.2Ueq(C & N). The H atom of the partially occupied ethanol solvent was included in a calculated position with O—H = 0.84Å and Uiso(H) = 1.1Ueq(O). The H atoms of the water molecules were located in difference Fourier maps and were refined with a distance restraint of 0.84 (2)Å and their isotropic displacement parameters were refined.

Computing details top

Data collection: RAPID-AUTO (Rigaku, 2004); cell refinement: RAPID-AUTO (Rigaku, 2004); data reduction: RAPID-AUTO (Rigaku, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL (Sheldrick, 1997b).

Figures top
[Figure 1] Fig. 1. A section of a one-dimensional chain of the title compound showing 30% probability displacement ellipsoids. All solvent molecules have been omitted.
[Figure 2] Fig. 2. The packing of title structure, showing hydrogen bonds as dashed lines.
catena-Poly[[[aqua(1,10-phenanthroline-κ2N,N')cadmium(II)]-µ- o-phenylenediacetato-κ2O,O':κO''-[bis(1,10-phenanthroline- κ2N,N')cadmium(II)]-µ-o-phenylenediacetato-κO:κ2O',O''] ethanol 0.79-solvate 3.05-hydrate] top
Crystal data top
[Cd2(C10H8O4)2(C12H8N2)3(H2O)]·0.79C2H6O·3.05H2OZ = 2
Mr = 1257.16F000 = 1274
Triclinic, P1Dx = 1.625 Mg m−3
Hall symbol: -P 1Mo Kα radiation
λ = 0.71073 Å
a = 12.6568 (2) ÅCell parameters from 21913 reflections
b = 14.7729 (3) Åθ = 3.0–27.5º
c = 15.0674 (3) ŵ = 0.90 mm−1
α = 68.710 (1)ºT = 153 (2) K
β = 83.896 (1)ºBlock, colorless
γ = 78.303 (1)º0.20 × 0.16 × 0.11 mm
V = 2568.84 (9) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer		10285 reflections with I > 2σ(I)
Radiation source: Rotating AnodeRint = 0.016
Monochromator: graphiteθmax = 27.5º
T = 153(2) Kθmin = 3.0º
ω scansh = −16→16
Absorption correction: nonek = −19→19
25428 measured reflectionsl = −19→19
11681 independent reflections
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)] = 0.025H atoms treated by a mixture of
independent and constrained refinement
wR(F2) = 0.093  w = 1/[σ2(Fo2) + (0.0676P)2 + 0.93P]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max = 0.001
11681 reflectionsΔρmax = 0.82 e Å−3
744 parametersΔρmin = −0.85 e Å−3
9 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997a), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0017 (3)
Crystal data top
[Cd2(C10H8O4)2(C12H8N2)3(H2O)]·0.79C2H6O·3.05H2Oγ = 78.303 (1)º
Mr = 1257.16V = 2568.84 (9) Å3
Triclinic, P1Z = 2
a = 12.6568 (2) ÅMo Kα
b = 14.7729 (3) ŵ = 0.90 mm−1
c = 15.0674 (3) ÅT = 153 (2) K
α = 68.710 (1)º0.20 × 0.16 × 0.11 mm
β = 83.896 (1)º
Data collection top
Rigaku R-AXIS RAPID
diffractometer		11681 independent reflections
Absorption correction: none10285 reflections with I > 2σ(I)
25428 measured reflectionsRint = 0.016
Refinement top
R[F2 > 2σ(F2)] = 0.0259 restraints
wR(F2) = 0.093H atoms treated by a mixture of
independent and constrained refinement
S = 1.01Δρmax = 0.82 e Å−3
11681 reflectionsΔρmin = −0.85 e Å−3
744 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)
Cd10.689294 (11)0.421799 (11)0.608438 (11)0.02153 (6)
Cd20.053959 (11)0.793489 (11)0.773349 (10)0.02087 (6)
O10.49865 (13)0.49043 (12)0.63061 (12)0.0290 (3)
O20.61249 (13)0.45434 (12)0.74444 (12)0.0296 (3)
O30.22400 (12)0.79301 (12)0.71617 (11)0.0253 (3)
O40.20909 (13)0.70938 (13)0.62286 (13)0.0324 (4)
O50.78141 (15)0.26364 (13)0.67143 (16)0.0418 (5)
O60.60941 (16)0.26266 (14)0.66945 (18)0.0471 (5)
O70.98151 (13)−0.07694 (12)0.65385 (12)0.0287 (3)
O81.02815 (15)0.03295 (15)0.70485 (15)0.0399 (4)
O90.68968 (15)0.41970 (15)0.45880 (14)0.0365 (4)
N10.85996 (15)0.45969 (14)0.61669 (13)0.0243 (4)
N20.69086 (15)0.59301 (14)0.51893 (14)0.0253 (4)
N3−0.08039 (15)0.72071 (13)0.74069 (13)0.0233 (4)
N40.09081 (15)0.61537 (14)0.85106 (14)0.0249 (4)
N5−0.08516 (17)0.84413 (15)0.88096 (15)0.0304 (4)
N60.13219 (18)0.80485 (15)0.90742 (14)0.0301 (4)
C10.51985 (18)0.48876 (16)0.71056 (17)0.0249 (4)
C20.43193 (19)0.52965 (17)0.77025 (17)0.0293 (5)
H2A0.36410.55450.73510.035*
H2B0.41860.47580.83040.035*
C30.46247 (17)0.61267 (18)0.79344 (17)0.0274 (5)
C40.5117 (2)0.5908 (2)0.8791 (2)0.0435 (7)
H40.52670.52420.92130.052*
C50.5390 (2)0.6647 (3)0.9037 (3)0.0588 (11)
H50.57120.64880.96290.071*
C60.5195 (2)0.7610 (3)0.8422 (3)0.0551 (10)
H60.53830.81180.85870.066*
C70.47280 (19)0.7833 (2)0.7570 (2)0.0399 (6)
H70.46020.84990.71460.048*
C80.44330 (16)0.71033 (17)0.73112 (17)0.0264 (5)
C90.38516 (17)0.73898 (17)0.64020 (16)0.0258 (4)
H9A0.41140.68910.60970.031*
H9B0.40120.80330.59570.031*
C100.26244 (17)0.74676 (16)0.65953 (15)0.0232 (4)
C110.7039 (2)0.21884 (17)0.68541 (18)0.0291 (5)
C120.7269 (2)0.10595 (17)0.72501 (18)0.0295 (5)
H12A0.80170.08270.74750.035*
H12B0.67710.08190.78020.035*
C130.71312 (17)0.06376 (15)0.64981 (16)0.0237 (4)
C140.61860 (18)0.02941 (17)0.65013 (17)0.0283 (5)
H140.56470.03020.69890.034*
C150.60195 (19)−0.00598 (17)0.58005 (18)0.0299 (5)
H150.5368−0.02880.58090.036*
C160.6798 (2)−0.00801 (17)0.50930 (18)0.0306 (5)
H160.6682−0.03150.46080.037*
C170.77596 (19)0.02477 (17)0.50944 (16)0.0280 (5)
H170.83000.02270.46100.034*
C180.79385 (17)0.06027 (15)0.57926 (16)0.0244 (4)
C190.90071 (18)0.09020 (16)0.58026 (18)0.0282 (5)
H19A0.88790.15130.59560.034*
H19B0.93600.10470.51600.034*
C200.97616 (17)0.00966 (17)0.65299 (17)0.0260 (4)
C210.94063 (19)0.39586 (18)0.66638 (17)0.0296 (5)
H210.93100.32960.69950.035*
C221.03977 (19)0.4216 (2)0.67239 (18)0.0340 (5)
H221.09520.37380.70970.041*
C231.05560 (19)0.5164 (2)0.62381 (18)0.0344 (5)
H231.12210.53520.62710.041*
C240.97165 (19)0.58586 (19)0.56868 (17)0.0295 (5)
C250.9833 (2)0.6857 (2)0.5142 (2)0.0354 (5)
H251.04870.70710.51570.042*
C260.9022 (2)0.74954 (19)0.4609 (2)0.0358 (5)
H260.91250.81460.42300.043*
C270.8011 (2)0.72061 (17)0.46086 (17)0.0290 (5)
C280.7118 (2)0.78729 (18)0.41059 (19)0.0359 (5)
H280.71850.85330.37260.043*
C290.6160 (2)0.7556 (2)0.4174 (2)0.0391 (6)
H290.55490.79980.38560.047*
C300.6090 (2)0.65751 (19)0.47168 (19)0.0320 (5)
H300.54240.63610.47480.038*
C310.78632 (18)0.62377 (16)0.51401 (16)0.0237 (4)
C320.87444 (17)0.55413 (17)0.56788 (16)0.0237 (4)
C33−0.16356 (18)0.77187 (17)0.68545 (16)0.0263 (4)
H33−0.16260.83910.64790.032*
C34−0.25225 (19)0.73094 (19)0.68023 (18)0.0297 (5)
H34−0.31020.77020.64050.036*
C35−0.25462 (19)0.63431 (19)0.73267 (17)0.0292 (5)
H35−0.31490.60580.73080.035*
C36−0.16710 (19)0.57734 (17)0.78951 (16)0.0262 (4)
C37−0.1615 (2)0.47415 (19)0.84237 (18)0.0329 (5)
H37−0.22000.44280.84220.040*
C38−0.0735 (2)0.42123 (18)0.89247 (18)0.0349 (5)
H38−0.07060.35260.92620.042*
C390.0153 (2)0.46562 (17)0.89621 (17)0.0294 (5)
C400.1087 (2)0.41219 (18)0.9472 (2)0.0383 (6)
H400.11540.34310.98050.046*
C410.1895 (2)0.4603 (2)0.9484 (2)0.0391 (6)
H410.25320.42500.98200.047*
C420.17758 (19)0.56245 (19)0.89955 (18)0.0320 (5)
H420.23420.59520.90130.038*
C430.01141 (18)0.56768 (16)0.84802 (15)0.0232 (4)
C44−0.08122 (17)0.62421 (16)0.79162 (15)0.0221 (4)
C45−0.1902 (2)0.8629 (2)0.8677 (2)0.0384 (6)
H45−0.21450.85350.81460.046*
C46−0.2673 (3)0.8960 (2)0.9283 (2)0.0487 (7)
H46−0.34210.90870.91660.058*
C47−0.2321 (3)0.9095 (3)1.0047 (2)0.0544 (8)
H47−0.28290.93251.04630.065*
C48−0.1213 (3)0.8896 (2)1.0217 (2)0.0448 (7)
C49−0.0793 (3)0.8993 (3)1.1015 (2)0.0560 (9)
H49−0.12790.92251.14430.067*
C500.0272 (3)0.8765 (3)1.1178 (2)0.0528 (8)
H500.05260.88251.17220.063*
C510.1025 (3)0.8431 (2)1.0527 (2)0.0421 (6)
C520.2130 (3)0.8170 (3)1.0670 (2)0.0517 (8)
H520.24130.82041.12140.062*
C530.2808 (3)0.7866 (3)1.0024 (2)0.0490 (7)
H530.35640.76871.01130.059*
C540.2367 (2)0.7823 (2)0.92304 (19)0.0370 (6)
H540.28440.76210.87800.044*
C550.0641 (2)0.83559 (17)0.97167 (17)0.0307 (5)
C56−0.0501 (2)0.85692 (17)0.95655 (18)0.0325 (5)
O111.24607 (16)−0.02220 (14)0.72639 (15)0.0380 (4)
O12−0.3976 (3)0.9918 (3)1.1718 (3)0.0813 (9)
O13−0.4695 (4)1.0800 (4)0.9987 (4)0.112 (2)0.846 (12)
O10−0.4680 (3)0.8163 (3)1.1848 (3)0.0728 (10)0.792 (4)
H10−0.50960.79441.23180.080*0.792 (4)
C58−0.4086 (5)0.7355 (4)1.1573 (5)0.115 (3)0.792 (4)
H58A−0.38460.76151.08950.137*0.792 (4)
H58B−0.45710.68851.16360.137*0.792 (4)
C57−0.3117 (5)0.6815 (5)1.2168 (6)0.121 (3)0.792 (4)
H57A−0.26270.72741.20990.133*0.792 (4)
H57B−0.27410.62781.19530.133*0.792 (4)
H57C−0.33510.65411.28380.133*0.792 (4)
O10W−0.4956 (12)0.7129 (10)1.1176 (10)0.0728 (10)0.208 (4)
H9AO0.720 (2)0.3728 (16)0.444 (2)0.035 (8)*
H9BO0.6380 (19)0.454 (2)0.428 (2)0.046 (9)*
H01A1.1821 (14)0.001 (3)0.716 (3)0.090 (16)*
H01B1.255 (3)−0.0762 (14)0.720 (3)0.055 (10)*
H02A−0.388 (3)0.9327 (8)1.194 (2)0.035 (9)*
H02B−0.363 (4)1.013 (4)1.201 (4)0.12 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.02012 (9)0.01939 (9)0.02826 (10)−0.00338 (6)−0.00033 (6)−0.01231 (7)
Cd20.02013 (9)0.01867 (9)0.02286 (9)−0.00310 (6)0.00037 (6)−0.00666 (6)
O10.0257 (7)0.0303 (8)0.0330 (9)−0.0016 (7)−0.0018 (6)−0.0150 (7)
O20.0261 (8)0.0292 (8)0.0339 (9)0.0007 (7)−0.0021 (6)−0.0142 (7)
O30.0217 (7)0.0269 (8)0.0292 (8)−0.0026 (6)0.0023 (6)−0.0137 (7)
O40.0250 (8)0.0390 (9)0.0403 (10)−0.0025 (7)−0.0031 (7)−0.0234 (8)
O50.0389 (10)0.0234 (8)0.0653 (13)−0.0052 (8)−0.0126 (9)−0.0155 (9)
O60.0359 (10)0.0292 (9)0.0783 (15)0.0020 (8)−0.0095 (10)−0.0233 (10)
O70.0275 (8)0.0199 (7)0.0335 (9)−0.0013 (6)−0.0038 (7)−0.0042 (7)
O80.0361 (9)0.0392 (10)0.0492 (11)−0.0002 (8)−0.0122 (8)−0.0218 (9)
O90.0324 (9)0.0444 (10)0.0418 (10)0.0077 (8)−0.0110 (8)−0.0307 (9)
N10.0229 (8)0.0278 (9)0.0242 (9)−0.0046 (7)−0.0009 (7)−0.0112 (8)
N20.0256 (9)0.0238 (9)0.0289 (10)−0.0055 (7)−0.0011 (7)−0.0112 (8)
N30.0236 (8)0.0215 (8)0.0251 (9)−0.0042 (7)−0.0017 (7)−0.0080 (7)
N40.0245 (9)0.0233 (9)0.0244 (9)−0.0007 (7)0.0000 (7)−0.0075 (8)
N50.0377 (11)0.0227 (9)0.0291 (10)−0.0059 (8)0.0061 (8)−0.0089 (8)
N60.0409 (11)0.0250 (9)0.0253 (10)−0.0108 (8)0.0032 (8)−0.0082 (8)
C10.0258 (10)0.0164 (9)0.0318 (11)−0.0054 (8)0.0040 (9)−0.0081 (9)
C20.0290 (11)0.0248 (11)0.0314 (12)−0.0053 (9)0.0081 (9)−0.0089 (9)
C30.0214 (10)0.0338 (12)0.0288 (11)−0.0002 (9)0.0024 (8)−0.0167 (10)
C40.0361 (13)0.0577 (18)0.0336 (13)0.0140 (13)−0.0068 (11)−0.0226 (13)
C50.0310 (13)0.105 (3)0.059 (2)0.0126 (17)−0.0159 (13)−0.060 (2)
C60.0233 (12)0.083 (2)0.089 (3)−0.0018 (14)−0.0059 (14)−0.069 (2)
C70.0214 (10)0.0419 (14)0.0691 (19)−0.0071 (10)0.0031 (11)−0.0348 (14)
C80.0162 (9)0.0288 (11)0.0392 (13)−0.0021 (8)0.0024 (8)−0.0195 (10)
C90.0218 (10)0.0245 (10)0.0293 (11)−0.0029 (8)0.0049 (8)−0.0097 (9)
C100.0230 (9)0.0197 (9)0.0239 (10)−0.0006 (8)0.0010 (8)−0.0065 (8)
C110.0337 (12)0.0251 (11)0.0328 (12)−0.0030 (9)−0.0051 (9)−0.0153 (10)
C120.0342 (12)0.0249 (11)0.0312 (12)−0.0048 (9)−0.0037 (9)−0.0116 (10)
C130.0255 (10)0.0166 (9)0.0277 (11)−0.0021 (8)−0.0037 (8)−0.0066 (8)
C140.0244 (10)0.0231 (10)0.0342 (12)−0.0033 (9)0.0002 (9)−0.0072 (9)
C150.0281 (11)0.0254 (11)0.0358 (12)−0.0077 (9)−0.0075 (9)−0.0069 (10)
C160.0371 (12)0.0237 (11)0.0319 (12)−0.0020 (9)−0.0119 (10)−0.0098 (10)
C170.0301 (11)0.0227 (10)0.0264 (11)0.0004 (9)0.0002 (9)−0.0062 (9)
C180.0222 (9)0.0153 (9)0.0315 (11)−0.0014 (8)−0.0034 (8)−0.0034 (8)
C190.0251 (10)0.0185 (10)0.0360 (12)−0.0054 (8)−0.0017 (9)−0.0028 (9)
C200.0200 (9)0.0251 (10)0.0293 (11)−0.0044 (8)0.0027 (8)−0.0062 (9)
C210.0275 (11)0.0306 (11)0.0306 (12)−0.0050 (9)−0.0018 (9)−0.0106 (10)
C220.0247 (11)0.0445 (14)0.0332 (12)−0.0025 (10)−0.0035 (9)−0.0152 (11)
C230.0231 (10)0.0506 (15)0.0350 (13)−0.0109 (10)0.0033 (9)−0.0203 (12)
C240.0271 (11)0.0372 (13)0.0289 (11)−0.0108 (10)0.0054 (9)−0.0160 (10)
C250.0323 (12)0.0377 (13)0.0430 (14)−0.0183 (11)0.0055 (10)−0.0178 (12)
C260.0435 (14)0.0293 (12)0.0394 (14)−0.0183 (11)0.0058 (11)−0.0134 (11)
C270.0342 (12)0.0254 (11)0.0313 (12)−0.0094 (9)0.0040 (9)−0.0137 (10)
C280.0466 (14)0.0212 (11)0.0379 (13)−0.0061 (10)−0.0002 (11)−0.0083 (10)
C290.0366 (13)0.0293 (12)0.0463 (15)0.0000 (11)−0.0068 (11)−0.0091 (12)
C300.0278 (11)0.0283 (12)0.0382 (13)−0.0026 (10)−0.0049 (10)−0.0099 (10)
C310.0271 (10)0.0242 (10)0.0241 (10)−0.0062 (8)0.0013 (8)−0.0134 (9)
C320.0242 (10)0.0279 (11)0.0242 (10)−0.0094 (9)0.0022 (8)−0.0136 (9)
C330.0272 (10)0.0224 (10)0.0279 (11)−0.0010 (9)−0.0036 (8)−0.0083 (9)
C340.0245 (10)0.0342 (12)0.0324 (12)−0.0010 (9)−0.0042 (9)−0.0155 (10)
C350.0261 (10)0.0359 (12)0.0323 (12)−0.0092 (10)0.0015 (9)−0.0185 (10)
C360.0328 (11)0.0267 (11)0.0229 (10)−0.0110 (9)0.0040 (8)−0.0113 (9)
C370.0427 (13)0.0299 (12)0.0309 (12)−0.0175 (10)0.0025 (10)−0.0112 (10)
C380.0518 (15)0.0201 (10)0.0315 (12)−0.0128 (10)0.0007 (11)−0.0048 (9)
C390.0396 (12)0.0207 (10)0.0265 (11)−0.0043 (9)0.0000 (9)−0.0075 (9)
C400.0480 (15)0.0199 (11)0.0378 (14)0.0028 (10)−0.0048 (11)−0.0029 (10)
C410.0354 (13)0.0343 (13)0.0387 (14)0.0091 (11)−0.0084 (11)−0.0085 (11)
C420.0253 (11)0.0318 (12)0.0360 (13)0.0007 (10)−0.0035 (9)−0.0107 (10)
C430.0277 (10)0.0206 (10)0.0200 (10)−0.0025 (8)0.0021 (8)−0.0075 (8)
C440.0265 (10)0.0209 (9)0.0203 (10)−0.0054 (8)0.0016 (8)−0.0089 (8)
C450.0406 (14)0.0369 (13)0.0382 (14)−0.0075 (11)0.0071 (11)−0.0159 (12)
C460.0420 (15)0.0547 (18)0.0521 (18)−0.0080 (14)0.0146 (13)−0.0268 (15)
C470.0562 (18)0.060 (2)0.0553 (19)−0.0157 (16)0.0265 (15)−0.0350 (17)
C480.0592 (18)0.0409 (15)0.0430 (15)−0.0206 (14)0.0193 (13)−0.0246 (13)
C490.076 (2)0.065 (2)0.0465 (17)−0.0284 (18)0.0256 (16)−0.0413 (17)
C500.077 (2)0.061 (2)0.0393 (16)−0.0317 (18)0.0136 (15)−0.0335 (15)
C510.0629 (18)0.0391 (14)0.0341 (14)−0.0238 (13)0.0078 (12)−0.0191 (12)
C520.066 (2)0.065 (2)0.0375 (15)−0.0264 (17)−0.0035 (14)−0.0253 (15)
C530.0491 (16)0.065 (2)0.0400 (16)−0.0140 (15)−0.0048 (13)−0.0233 (15)
C540.0410 (13)0.0420 (14)0.0295 (12)−0.0111 (12)0.0003 (10)−0.0128 (11)
C550.0483 (14)0.0223 (10)0.0256 (11)−0.0158 (10)0.0070 (10)−0.0104 (9)
C560.0494 (14)0.0226 (11)0.0285 (12)−0.0154 (10)0.0106 (10)−0.0111 (9)
O110.0382 (10)0.0286 (9)0.0483 (11)−0.0083 (8)0.0015 (8)−0.0143 (8)
O120.088 (2)0.087 (2)0.100 (2)−0.0421 (19)0.0266 (18)−0.065 (2)
O130.098 (3)0.112 (4)0.133 (4)−0.023 (3)−0.035 (3)−0.039 (3)
O100.083 (2)0.067 (2)0.073 (2)−0.0356 (18)0.0166 (18)−0.0234 (18)
C580.165 (8)0.113 (6)0.091 (5)−0.092 (6)0.021 (5)−0.036 (5)
C570.088 (5)0.176 (9)0.155 (8)−0.045 (5)0.036 (5)−0.122 (7)
O10W0.083 (2)0.067 (2)0.073 (2)−0.0356 (18)0.0166 (18)−0.0234 (18)
Geometric parameters (Å, °) top
Cd1—O92.2656 (18)C21—C221.404 (3)
Cd1—O52.2891 (18)C21—H210.9500
Cd1—O22.3404 (16)C22—C231.369 (4)
Cd1—N12.3649 (19)C22—H220.9500
Cd1—N22.399 (2)C23—C241.414 (3)
Cd1—O12.4586 (15)C23—H230.9500
Cd1—O62.567 (2)C24—C321.405 (3)
Cd1—C12.737 (2)C24—C251.433 (4)
Cd2—O7i2.2098 (16)C25—C261.349 (4)
Cd2—O32.2312 (15)C25—H250.9500
Cd2—N32.3650 (19)C26—C271.430 (4)
Cd2—N62.414 (2)C26—H260.9500
Cd2—N42.4277 (19)C27—C311.403 (3)
Cd2—N52.455 (2)C27—C281.417 (4)
O1—C11.252 (3)C28—C291.367 (4)
O2—C11.261 (3)C28—H280.9500
O3—C101.278 (3)C29—C301.397 (4)
O4—C101.232 (3)C29—H290.9500
O5—C111.251 (3)C30—H300.9500
O6—C111.241 (3)C31—C321.443 (3)
O7—C201.263 (3)C33—C341.400 (3)
O7—Cd2ii2.2099 (16)C33—H330.9500
O8—C201.248 (3)C34—C351.362 (4)
O9—H9AO0.81 (3)C34—H340.9500
O9—H9BO0.81 (3)C35—C361.403 (3)
N1—C211.324 (3)C35—H350.9500
N1—C321.360 (3)C36—C441.411 (3)
N2—C301.324 (3)C36—C371.432 (3)
N2—C311.360 (3)C37—C381.349 (4)
N3—C331.334 (3)C37—H370.9500
N3—C441.353 (3)C38—C391.427 (4)
N4—C421.326 (3)C38—H380.9500
N4—C431.352 (3)C39—C431.409 (3)
N5—C451.324 (4)C39—C401.409 (4)
N5—C561.352 (3)C40—C411.364 (4)
N6—C541.322 (3)C40—H400.9500
N6—C551.367 (3)C41—C421.402 (4)
C1—C21.524 (3)C41—H410.9500
C2—C31.519 (3)C42—H420.9500
C2—H2A0.9900C43—C441.447 (3)
C2—H2B0.9900C45—C461.402 (4)
C3—C81.394 (3)C45—H450.9500
C3—C41.395 (3)C46—C471.369 (5)
C4—C51.387 (5)C46—H460.9500
C4—H40.9500C47—C481.406 (5)
C5—C61.376 (6)C47—H470.9500
C5—H50.9500C48—C561.410 (3)
C6—C71.372 (5)C48—C491.428 (5)
C6—H60.9500C49—C501.348 (5)
C7—C81.398 (3)C49—H490.9500
C7—H70.9500C50—C511.441 (4)
C8—C91.505 (3)C50—H500.9500
C9—C101.538 (3)C51—C521.392 (5)
C9—H9A0.9900C51—C551.409 (4)
C9—H9B0.9900C52—C531.367 (4)
C11—C121.529 (3)C52—H520.9500
C12—C131.517 (3)C53—C541.399 (4)
C12—H12A0.9900C53—H530.9500
C12—H12B0.9900C54—H540.9500
C13—C141.390 (3)C55—C561.439 (4)
C13—C181.401 (3)O11—H01A0.82 (3)
C14—C151.388 (3)O11—H01B0.82 (3)
C14—H140.9500O12—O132.624 (6)
C15—C161.377 (4)O12—H02A0.80 (3)
C15—H150.9500O12—H02B0.83 (6)
C16—C171.399 (4)O10—C581.446 (3)
C16—H160.9500O10—H100.8400
C17—C181.390 (3)C58—C571.504 (3)
C17—H170.9500C58—H58A0.9900
C18—C191.509 (3)C58—H58B0.9900
C19—C201.531 (3)C57—H57A0.9800
C19—H19A0.9900C57—H57B0.9800
C19—H19B0.9900C57—H57C0.9800
O9—Cd1—O594.96 (7)C16—C17—H17119.4
O9—Cd1—O2155.26 (6)C17—C18—C13118.9 (2)
O5—Cd1—O2102.44 (7)C17—C18—C19119.8 (2)
O9—Cd1—N1103.79 (7)C13—C18—C19121.3 (2)
O5—Cd1—N181.95 (7)C18—C19—C20112.13 (18)
O2—Cd1—N196.01 (6)C18—C19—H19A109.2
O9—Cd1—N280.43 (7)C20—C19—H19A109.2
O5—Cd1—N2149.43 (7)C18—C19—H19B109.2
O2—Cd1—N292.79 (6)C20—C19—H19B109.2
N1—Cd1—N270.09 (6)H19A—C19—H19B107.9
O9—Cd1—O1100.71 (6)O8—C20—O7125.1 (2)
O5—Cd1—O1130.02 (7)O8—C20—C19119.4 (2)
O2—Cd1—O154.58 (5)O7—C20—C19115.5 (2)
N1—Cd1—O1137.32 (6)N1—C21—C22123.0 (2)
N2—Cd1—O180.34 (6)N1—C21—H21118.5
O9—Cd1—O688.46 (8)C22—C21—H21118.5
O5—Cd1—O653.06 (6)C23—C22—C21119.2 (2)
O2—Cd1—O688.12 (7)C23—C22—H22120.4
N1—Cd1—O6134.45 (6)C21—C22—H22120.4
N2—Cd1—O6155.23 (6)C22—C23—C24119.1 (2)
O1—Cd1—O680.08 (6)C22—C23—H23120.4
O9—Cd1—C1127.90 (7)C24—C23—H23120.4
O5—Cd1—C1119.58 (7)C32—C24—C23117.8 (2)
O2—Cd1—C127.37 (6)C32—C24—C25119.9 (2)
N1—Cd1—C1117.77 (7)C23—C24—C25122.3 (2)
N2—Cd1—C185.39 (6)C26—C25—C24120.7 (2)
O1—Cd1—C127.23 (6)C26—C25—H25119.6
O6—Cd1—C184.13 (7)C24—C25—H25119.6
O7i—Cd2—O396.07 (6)C25—C26—C27120.8 (2)
O7i—Cd2—N382.72 (6)C25—C26—H26119.6
O3—Cd2—N3128.91 (6)C27—C26—H26119.6
O7i—Cd2—N6123.74 (7)C31—C27—C28117.4 (2)
O3—Cd2—N681.73 (6)C31—C27—C26120.0 (2)
N3—Cd2—N6139.90 (7)C28—C27—C26122.5 (2)
O7i—Cd2—N4148.45 (7)C29—C28—C27119.2 (2)
O3—Cd2—N490.95 (6)C29—C28—H28120.4
N3—Cd2—N469.16 (6)C27—C28—H28120.4
N6—Cd2—N487.67 (7)C28—C29—C30119.3 (2)
O7i—Cd2—N588.72 (7)C28—C29—H29120.3
O3—Cd2—N5146.51 (7)C30—C29—H29120.3
N3—Cd2—N584.56 (7)N2—C30—C29123.1 (2)
N6—Cd2—N568.34 (7)N2—C30—H30118.5
N4—Cd2—N5102.12 (6)C29—C30—H30118.5
C1—O1—Cd188.85 (13)N2—C31—C27122.6 (2)
C1—O2—Cd194.08 (14)N2—C31—C32118.2 (2)
C10—O3—Cd2120.91 (14)C27—C31—C32119.2 (2)
C11—O5—Cd198.65 (15)N1—C32—C24122.3 (2)
C11—O6—Cd185.81 (16)N1—C32—C31118.5 (2)
C20—O7—Cd2ii121.04 (15)C24—C32—C31119.2 (2)
Cd1—O9—H9AO122 (2)N3—C33—C34123.0 (2)
Cd1—O9—H9BO115 (2)N3—C33—H33118.5
H9AO—O9—H9BO118 (3)C34—C33—H33118.5
C21—N1—C32118.5 (2)C35—C34—C33119.4 (2)
C21—N1—Cd1124.41 (17)C35—C34—H34120.3
C32—N1—Cd1117.07 (14)C33—C34—H34120.3
C30—N2—C31118.3 (2)C34—C35—C36119.3 (2)
C30—N2—Cd1125.61 (17)C34—C35—H35120.4
C31—N2—Cd1116.00 (14)C36—C35—H35120.4
C33—N3—C44118.0 (2)C35—C36—C44117.9 (2)
C33—N3—Cd2123.73 (15)C35—C36—C37122.2 (2)
C44—N3—Cd2117.61 (14)C44—C36—C37119.8 (2)
C42—N4—C43118.0 (2)C38—C37—C36120.2 (2)
C42—N4—Cd2126.33 (18)C38—C37—H37119.9
C43—N4—Cd2115.59 (14)C36—C37—H37119.9
C45—N5—C56118.8 (2)C37—C38—C39121.7 (2)
C45—N5—Cd2124.48 (17)C37—C38—H38119.1
C56—N5—Cd2116.65 (17)C39—C38—H38119.1
C54—N6—C55118.0 (2)C43—C39—C40117.0 (2)
C54—N6—Cd2124.04 (16)C43—C39—C38119.9 (2)
C55—N6—Cd2117.99 (17)C40—C39—C38123.1 (2)
O1—C1—O2122.4 (2)C41—C40—C39119.6 (2)
O1—C1—C2119.8 (2)C41—C40—H40120.2
O2—C1—C2117.8 (2)C39—C40—H40120.2
O1—C1—Cd163.93 (11)C40—C41—C42119.3 (2)
O2—C1—Cd158.55 (11)C40—C41—H41120.4
C2—C1—Cd1175.33 (17)C42—C41—H41120.4
C3—C2—C1112.04 (19)N4—C42—C41123.0 (3)
C3—C2—H2A109.2N4—C42—H42118.5
C1—C2—H2A109.2C41—C42—H42118.5
C3—C2—H2B109.2N4—C43—C39123.1 (2)
C1—C2—H2B109.2N4—C43—C44118.24 (19)
H2A—C2—H2B107.9C39—C43—C44118.6 (2)
C8—C3—C4118.9 (2)N3—C44—C36122.5 (2)
C8—C3—C2121.8 (2)N3—C44—C43117.9 (2)
C4—C3—C2119.2 (2)C36—C44—C43119.6 (2)
C5—C4—C3121.0 (3)N5—C45—C46123.0 (3)
C5—C4—H4119.5N5—C45—H45118.5
C3—C4—H4119.5C46—C45—H45118.5
C6—C5—C4119.9 (3)C47—C46—C45118.5 (3)
C6—C5—H5120.1C47—C46—H46120.8
C4—C5—H5120.1C45—C46—H46120.8
C7—C6—C5119.7 (3)C46—C47—C48120.3 (3)
C7—C6—H6120.2C46—C47—H47119.9
C5—C6—H6120.2C48—C47—H47119.9
C6—C7—C8121.5 (3)C47—C48—C56117.0 (3)
C6—C7—H7119.2C47—C48—C49123.2 (3)
C8—C7—H7119.2C56—C48—C49119.7 (3)
C3—C8—C7119.0 (2)C50—C49—C48121.9 (3)
C3—C8—C9121.2 (2)C50—C49—H49119.0
C7—C8—C9119.7 (2)C48—C49—H49119.0
C8—C9—C10111.10 (18)C49—C50—C51119.9 (3)
C8—C9—H9A109.4C49—C50—H50120.0
C10—C9—H9A109.4C51—C50—H50120.0
C8—C9—H9B109.4C52—C51—C55118.1 (3)
C10—C9—H9B109.4C52—C51—C50122.4 (3)
H9A—C9—H9B108.0C55—C51—C50119.6 (3)
O4—C10—O3124.9 (2)C53—C52—C51119.8 (3)
O4—C10—C9120.84 (19)C53—C52—H52120.1
O3—C10—C9114.27 (19)C51—C52—H52120.1
O6—C11—O5122.4 (2)C52—C53—C54118.7 (3)
O6—C11—C12119.2 (2)C52—C53—H53120.6
O5—C11—C12118.4 (2)C54—C53—H53120.6
C13—C12—C11111.20 (19)N6—C54—C53123.5 (3)
C13—C12—H12A109.4N6—C54—H54118.2
C11—C12—H12A109.4C53—C54—H54118.2
C13—C12—H12B109.4N6—C55—C51121.9 (3)
C11—C12—H12B109.4N6—C55—C56118.0 (2)
H12A—C12—H12B108.0C51—C55—C56120.0 (2)
C14—C13—C18119.6 (2)N5—C56—C48122.4 (3)
C14—C13—C12119.6 (2)N5—C56—C55118.9 (2)
C18—C13—C12120.8 (2)C48—C56—C55118.7 (2)
C15—C14—C13120.8 (2)H01A—O11—H01B105 (4)
C15—C14—H14119.6O13—O12—H02A119 (3)
C13—C14—H14119.6O13—O12—H02B128 (5)
C16—C15—C14120.1 (2)H02A—O12—H02B110 (5)
C16—C15—H15120.0O10—C58—C57112.6 (3)
C14—C15—H15120.0O10—C58—H58A109.1
C15—C16—C17119.4 (2)C57—C58—H58A109.1
C15—C16—H16120.3O10—C58—H58B109.1
C17—C16—H16120.3C57—C58—H58B109.1
C18—C17—C16121.1 (2)H58A—C58—H58B107.8
C18—C17—H17119.4
Symmetry codes: (i) x−1, y+1, z; (ii) x+1, y−1, z.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O9—H9BO···O1iii0.81 (3)1.92 (3)2.713 (2)167 (4)
O9—H9AO···O4iii0.81 (3)1.88 (3)2.678 (2)164 (3)
O11—H01B···O3ii0.82 (3)2.07 (3)2.860 (3)161 (4)
O11—H01A···O80.82 (3)1.92 (3)2.732 (3)170 (5)
O12—H02A···O100.80 (3)2.22 (3)2.844 (5)136 (3)
O12—H02B···O11iv0.83 (6)1.98 (5)2.776 (4)161 (6)
O10—H10···O6v0.841.912.745 (5)174
Symmetry codes: (iii) −x+1, −y+1, −z+1; (ii) x+1, y−1, z; (iv) −x+1, −y+1, −z+2; (v) −x, −y+1, −z+2.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O9—H9BO···O1i0.81 (3)1.92 (3)2.713 (2)167 (4)
O9—H9AO···O4i0.81 (3)1.88 (3)2.678 (2)164 (3)
O11—H01B···O3ii0.82 (3)2.07 (3)2.860 (3)161 (4)
O11—H01A···O80.82 (3)1.92 (3)2.732 (3)170 (5)
O12—H02A···O100.80 (3)2.22 (3)2.844 (5)136 (3)
O12—H02B···O11iii0.83 (6)1.98 (5)2.776 (4)161 (6)
O10—H10···O6iv0.841.912.745 (5)174
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1, y−1, z; (iii) −x+1, −y+1, −z+2; (iv) −x, −y+1, −z+2.
Acknowledgements top

We acknowledge financial support by the NSFC (Nos. 30460153 and 20561001) and the Natural Science Foundation of Guangxi Province (No. 0447019).

references
References top

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