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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 68| Part 4| April 2012| Pages m477-m478

catena-Poly[[bis­­(μ3-5-hy­dr­oxy­isophthalato)bis­­(pyrazino­[2,3-f][1,10]phenanthroline)dicadmium] dihydrate]

aDepartment of Forensic Chemistry, China Criminal Police University, Shenyang 110854, People's Republic of China
*Correspondence e-mail: zpcccpc@ccpc.edu.cn

(Received 11 December 2011; accepted 18 March 2012; online 24 March 2012)

The title coordination polymer, {[Cd2(C8H4O5)2(C14H8N4)2]·2H2O}n, has a layered structure. The asymmetric unit contains two CdII ions, two pyrazino­[2,3-f][1,10]phenanthroline, two 5-hy­droxy­isophthalate (hip) ligands and two lattice water mol­ecules. Each CdII ion is coordinated by two N atoms from a chelating pyrazino­[2,3-f][1,10]phenanthroline and four O atoms from three different hip ligands, resulting in a distorted CdN2O4 octa­hedral coordination environment. The hip ligand connects adjacent CdII ions, forming forming layers parallel to (010). Intralayer O—H⋯O hydrogen bonds involving the hydroxy groups and solvent water molecules consolidate the crystal packing.

Related literature

For metal–carboxyl­ate complexes containing a pyrazino­[2,3-f][1,10]phenanthroline ligand, see: He & Han (2006[He, Y.-K. & Han, Z.-B. (2006). Acta Cryst. E62, m2676-m2677.]); Han et al. (2009[Han, Z.-B., Ji, J.-W., An, H.-Y., Zhang, W., Han, G.-X., Zhang, G.-X. & Yang, L.-G. (2009). Dalton Trans. pp. 9807-9811.]); Wang et al. (2007[Wang, X.-L., Bi, Y. F., Lin, H. Y. & Liu, G. C. (2007). Cryst. Growth Des. 72, 1086-1091.]).

[Scheme 1]

Experimental

Crystal data
  • [Cd2(C8H4O5)2(C14H8N4)2]·2H2O

  • Mr = 1085.54

  • Triclinic, [P \overline 1]

  • a = 8.6754 (13) Å

  • b = 15.1114 (17) Å

  • c = 15.629 (3) Å

  • α = 92.903 (16)°

  • β = 97.143 (13)°

  • γ = 95.515 (9)°

  • V = 2019.6 (5) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 1.13 mm−1

  • T = 293 K

  • 0.37 × 0.33 × 0.27 mm

Data collection
  • Bruker APEX area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.681, Tmax = 0.751

  • 11100 measured reflections

  • 9275 independent reflections

  • 8147 reflections with I > 2σ(I)

  • Rint = 0.061

Refinement
  • R[F2 > 2σ(F2)] = 0.031

  • wR(F2) = 0.114

  • S = 1.07

  • 9275 reflections

  • 595 parameters

  • H-atom parameters constrained

  • Δρmax = 0.70 e Å−3

  • Δρmin = −1.43 e Å−3

Table 1
Selected bond lengths (Å)

Cd1—O7 2.205 (3)
Cd1—O1 2.259 (2)
Cd1—N2 2.339 (3)
Cd1—O4i 2.360 (2)
Cd1—N1 2.367 (3)
Cd1—O5i 2.384 (3)
Cd2—O2 2.202 (2)
Cd2—O6 2.295 (3)
Cd2—N5 2.325 (3)
Cd2—O9ii 2.332 (2)
Cd2—N6 2.343 (3)
Cd2—O10ii 2.362 (3)
Symmetry codes: (i) -x, -y, -z; (ii) -x+1, -y, -z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O3—H3B⋯O2Wiii 0.82 1.84 2.659 (4) 177
O8—H8A⋯O1Wiv 0.82 1.85 2.672 (4) 177
O1W—H1WA⋯O9v 0.85 2.14 2.912 (4) 150
O1W—H1WB⋯O2v 0.85 2.27 2.963 (4) 138
O2W—H2WA⋯O4vi 0.85 2.28 2.880 (4) 127
O2W—H2WB⋯O7vi 0.85 2.33 2.955 (4) 131
Symmetry codes: (iii) x, y-1, z; (iv) x-1, y-1, z; (v) x, y+1, z; (vi) x+1, y+1, z.

Data collection: SMART (Bruker, 2001[Bruker (2001). SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2001[Bruker (2001). SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; 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 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXL97.

Supporting information


Comment top

Recently, several metal-carboxylate complexes containing an N-donor chelate ligand TATP and its large analogue DPPZ dipyridophenazine have been reported (He & Han, 2006; Wang et al., 2007; Han et al., 2009). I report here a new one-dimensional CdII coordination polymer constructed by CdII ions, pyrazino[2,3-f][1,10]phenanthroline (TATP) and 5-hydroxyisophthalic acid (H2Hip), (I).

Complex (I) exhibits a layered structure in which the asymmetric unit consists of two CdII ions, two hip, two TATP ligand and two lattice water molecules (Fig. 1). Fig. 2 shows a fragment of the fragment of ribbon chain in the structure of I. Each CdII is hexa-coordinate and is surrounded by four oxygen atoms from three different hip ligands and two nitrogen atoms from a chelating TATP ligand (Table 1), forming a distorted octahedral geometry.

The hip ligand connects adjacent CdII ions, forming layers parallel to (010). Intralayer O—H···O hydrogen bonds involving the hydroxy groups and solvent water molecules consolidate the crystal packing. A face-to-face distance of 3.491 Å between a pair of TATP ligands coordinated to the two CdII ions is observed, showing significant ππ stacking interactions.

Related literature top

For metal–carboxylate complexes containing a pyrazino[2,3-f][1,10]phenanthroline ligand, see: He & Han (2006); Han et al. (2009); Wang et al. (2007)

Experimental top

A mixture of Cd(NO3)2.4H2O (0.5 mmol, 0.154 g), pyrazino[2,3-f][1,10]phenanthroline ligand (0.5 mmol, 0.116 g), H2hip (0.5 mmol, 0.083 g) and water (10 ml) was mixed in a 23 ml Teflon reactor, which was heated at 180° for six days and then cooled to room temperature at a rate of 5 ° h-1.Yield: 38%. CH&N analysis for C68H38Cu3N8 (found/calc): C, 48.68(48.97), H, 2.60(2.71), N, 10.32%(10.63%).

Refinement top

The H atoms of the aromatic rings were placed at calculated positions in the riding model approximation (C—H 0.93 Å) with their temperature factors were set to 1.2 times those of the equivalent isotropic temperature factors of the parent atoms. The hydroxy H atom was placed at calculated positions in the riding model approximation(O—H 0.82 Å) with their temperature factors were set to 1.2 times those of the equivalent isotropic temperature factors of the parent atoms.

Structure description top

Recently, several metal-carboxylate complexes containing an N-donor chelate ligand TATP and its large analogue DPPZ dipyridophenazine have been reported (He & Han, 2006; Wang et al., 2007; Han et al., 2009). I report here a new one-dimensional CdII coordination polymer constructed by CdII ions, pyrazino[2,3-f][1,10]phenanthroline (TATP) and 5-hydroxyisophthalic acid (H2Hip), (I).

Complex (I) exhibits a layered structure in which the asymmetric unit consists of two CdII ions, two hip, two TATP ligand and two lattice water molecules (Fig. 1). Fig. 2 shows a fragment of the fragment of ribbon chain in the structure of I. Each CdII is hexa-coordinate and is surrounded by four oxygen atoms from three different hip ligands and two nitrogen atoms from a chelating TATP ligand (Table 1), forming a distorted octahedral geometry.

The hip ligand connects adjacent CdII ions, forming layers parallel to (010). Intralayer O—H···O hydrogen bonds involving the hydroxy groups and solvent water molecules consolidate the crystal packing. A face-to-face distance of 3.491 Å between a pair of TATP ligands coordinated to the two CdII ions is observed, showing significant ππ stacking interactions.

For metal–carboxylate complexes containing a pyrazino[2,3-f][1,10]phenanthroline ligand, see: He & Han (2006); Han et al. (2009); Wang et al. (2007)

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXL97 (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. View of the structure of (I). Displacement ellipsoids are drawn at the 30% probability level. H atoms and the lattice water molecule have been omitted for clarity. [Symmetry code: (i) -x, -y + 1, -z + 1.]
[Figure 2] Fig. 2. The fragment of one-dimensional ribbon chain.
i>catena-Poly[[bis(µ3-5-hydroxyisophthalato)bis(pyrazino[2,3- f][1,10]phenanthroline)dicadmium] dihydrate] top
Crystal data top
[Cd2(C8H4O5)2(C14H8N4)2]·2H2OZ = 2
Mr = 1085.54F(000) = 1080
Triclinic, P1Dx = 1.785 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.6754 (13) ÅCell parameters from 20 reflections
b = 15.1114 (17) Åθ = 2.7–22.3°
c = 15.629 (3) ŵ = 1.13 mm1
α = 92.903 (16)°T = 293 K
β = 97.143 (13)°Block, red
γ = 95.515 (9)°0.37 × 0.33 × 0.27 mm
V = 2019.6 (5) Å3
Data collection top
Bruker APEX area-detector
diffractometer
9275 independent reflections
Radiation source: fine-focus sealed tube8147 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.061
φ and ω scanθmax = 27.5°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 111
Tmin = 0.681, Tmax = 0.751k = 1919
11100 measured reflectionsl = 2020
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)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.114H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0613P)2 + 2.6404P]
where P = (Fo2 + 2Fc2)/3
9275 reflections(Δ/σ)max = 0.009
595 parametersΔρmax = 0.70 e Å3
0 restraintsΔρmin = 1.43 e Å3
Crystal data top
[Cd2(C8H4O5)2(C14H8N4)2]·2H2Oγ = 95.515 (9)°
Mr = 1085.54V = 2019.6 (5) Å3
Triclinic, P1Z = 2
a = 8.6754 (13) ÅMo Kα radiation
b = 15.1114 (17) ŵ = 1.13 mm1
c = 15.629 (3) ÅT = 293 K
α = 92.903 (16)°0.37 × 0.33 × 0.27 mm
β = 97.143 (13)°
Data collection top
Bruker APEX area-detector
diffractometer
9275 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
8147 reflections with I > 2σ(I)
Tmin = 0.681, Tmax = 0.751Rint = 0.061
11100 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0310 restraints
wR(F2) = 0.114H-atom parameters constrained
S = 1.07Δρmax = 0.70 e Å3
9275 reflectionsΔρmin = 1.43 e Å3
595 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
Cd10.10447 (3)0.188967 (14)0.170325 (14)0.02701 (8)
Cd20.47056 (3)0.185064 (14)0.355404 (14)0.02830 (8)
C10.4157 (4)0.0769 (2)0.1864 (2)0.0325 (7)
C20.4157 (4)0.0043 (2)0.1274 (2)0.0293 (6)
C30.2868 (4)0.0312 (2)0.0662 (2)0.0298 (6)
H3A0.20470.00410.05780.036*
C40.2821 (4)0.1116 (2)0.0176 (2)0.0306 (6)
C50.4080 (4)0.1622 (2)0.0279 (2)0.0355 (7)
H5A0.40560.21510.00550.043*
C60.5372 (4)0.1341 (2)0.0879 (2)0.0359 (7)
C70.5410 (4)0.0553 (2)0.1379 (2)0.0327 (7)
H7A0.62720.03660.17850.039*
C80.1421 (4)0.1441 (2)0.0463 (2)0.0328 (7)
C90.1081 (4)0.0759 (2)0.3173 (2)0.0327 (7)
C100.0805 (4)0.0039 (2)0.3672 (2)0.0301 (6)
C110.0632 (4)0.0553 (2)0.3504 (2)0.0335 (7)
H11A0.14220.03710.31140.040*
C120.0887 (4)0.1337 (2)0.3918 (2)0.0355 (7)
C130.0304 (4)0.1612 (2)0.4484 (2)0.0362 (7)
H13A0.01430.21410.47550.043*
C140.1743 (4)0.1098 (2)0.4649 (2)0.0306 (6)
C150.1995 (4)0.0305 (2)0.4259 (2)0.0297 (6)
H15A0.29440.00470.43860.036*
C160.3017 (4)0.1412 (2)0.5267 (2)0.0314 (6)
C170.0218 (5)0.3044 (3)0.3270 (2)0.0407 (8)
H17A0.03250.24920.35060.049*
C180.0821 (6)0.3758 (3)0.3664 (3)0.0544 (11)
H18A0.13100.36860.41560.065*
C190.0680 (6)0.4571 (3)0.3312 (3)0.0565 (11)
H19A0.10640.50580.35680.068*
C200.0046 (5)0.4664 (2)0.2565 (3)0.0419 (8)
C210.0198 (5)0.5501 (3)0.2146 (3)0.0509 (10)
C220.0273 (9)0.6946 (3)0.2073 (5)0.090 (2)
H22A0.06830.74500.22790.108*
C230.0499 (9)0.6999 (3)0.1355 (6)0.097 (2)
H23A0.05810.75400.10980.117*
C240.0961 (6)0.5557 (3)0.1413 (3)0.0531 (11)
C250.1584 (5)0.4778 (3)0.1055 (3)0.0439 (9)
C260.2386 (7)0.4795 (4)0.0330 (3)0.0671 (14)
H26A0.25380.53200.00520.081*
C270.2944 (7)0.4036 (4)0.0034 (4)0.0712 (15)
H27A0.34960.40440.04400.085*
C280.2678 (5)0.3250 (3)0.0449 (3)0.0495 (10)
H28A0.30310.27310.02350.059*
C290.1410 (4)0.3973 (2)0.1447 (2)0.0329 (7)
C300.0625 (4)0.3913 (2)0.2218 (2)0.0317 (6)
C310.3204 (5)0.3164 (3)0.4855 (3)0.0500 (10)
H31A0.30560.26450.51430.060*
C320.2675 (6)0.3944 (4)0.5176 (4)0.0709 (15)
H32A0.21970.39450.56770.085*
C330.2864 (6)0.4703 (4)0.4750 (4)0.0718 (16)
H33A0.25030.52230.49540.086*
C340.3604 (5)0.4699 (3)0.4003 (3)0.0499 (10)
C350.3880 (6)0.5474 (3)0.3515 (4)0.0602 (14)
C360.3659 (10)0.6943 (4)0.3319 (7)0.105 (3)
H36A0.33230.74860.34820.126*
C370.4468 (10)0.6902 (4)0.2608 (6)0.104 (3)
H37A0.46660.74150.23180.125*
C380.4669 (6)0.5434 (3)0.2791 (3)0.0574 (12)
C390.5212 (5)0.4600 (2)0.2509 (3)0.0457 (9)
C400.6034 (6)0.4512 (3)0.1801 (3)0.0616 (13)
H40A0.62530.50000.14810.074*
C410.6517 (6)0.3701 (3)0.1580 (3)0.0574 (11)
H41A0.70900.36410.11190.069*
C420.6148 (5)0.2978 (3)0.2045 (2)0.0419 (8)
H42A0.64490.24280.18790.050*
C430.4924 (4)0.3842 (2)0.2967 (2)0.0331 (7)
C440.4124 (4)0.3889 (2)0.3731 (2)0.0331 (7)
N10.0498 (3)0.31172 (18)0.25765 (18)0.0313 (6)
N20.1936 (3)0.32205 (19)0.11392 (19)0.0347 (6)
N30.0450 (6)0.6199 (3)0.2481 (3)0.0731 (13)
N40.1131 (6)0.6324 (3)0.1010 (4)0.0768 (14)
N50.3913 (3)0.3145 (2)0.41515 (18)0.0341 (6)
N60.5371 (3)0.30456 (19)0.27266 (18)0.0320 (6)
N70.3338 (6)0.6247 (3)0.3780 (4)0.0876 (17)
N80.4967 (6)0.6145 (3)0.2330 (4)0.0839 (16)
O10.3399 (3)0.13916 (16)0.16202 (18)0.0387 (5)
O20.4944 (3)0.07607 (18)0.26051 (17)0.0445 (6)
O30.6581 (3)0.18602 (19)0.0963 (2)0.0507 (7)
H3B0.74090.15410.10700.076*
O40.0151 (3)0.11105 (18)0.04066 (16)0.0396 (6)
O50.1536 (3)0.2029 (2)0.10328 (18)0.0463 (7)
O60.2090 (3)0.13873 (17)0.34703 (19)0.0411 (6)
O70.0264 (3)0.07608 (18)0.24391 (18)0.0452 (6)
O80.2273 (3)0.1863 (2)0.3755 (2)0.0531 (8)
H8A0.29920.15480.36890.080*
O90.4413 (3)0.10890 (18)0.52495 (17)0.0418 (6)
O100.2685 (3)0.1985 (2)0.57699 (19)0.0488 (7)
O1W0.5320 (3)0.9117 (2)0.3532 (2)0.0517 (7)
H1WA0.48280.91970.39630.062*
H1WB0.57290.95620.32990.062*
O2W0.9326 (3)0.91177 (19)0.1314 (2)0.0482 (6)
H2WA0.99580.88620.10360.058*
H2WB0.93350.96810.13280.058*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.02968 (12)0.02234 (12)0.02818 (12)0.00372 (8)0.00040 (9)0.00180 (8)
Cd20.03162 (13)0.02485 (12)0.02733 (12)0.00397 (9)0.00178 (9)0.00298 (8)
C10.0262 (15)0.0321 (16)0.0382 (17)0.0037 (12)0.0032 (13)0.0048 (13)
C20.0280 (15)0.0315 (15)0.0284 (15)0.0067 (12)0.0022 (12)0.0014 (12)
C30.0294 (15)0.0305 (15)0.0298 (15)0.0079 (12)0.0011 (12)0.0012 (12)
C40.0290 (15)0.0341 (16)0.0281 (15)0.0040 (12)0.0019 (12)0.0021 (12)
C50.0362 (17)0.0334 (16)0.0359 (17)0.0079 (13)0.0015 (14)0.0088 (13)
C60.0283 (15)0.0396 (18)0.0401 (18)0.0119 (13)0.0013 (13)0.0032 (14)
C70.0272 (15)0.0364 (17)0.0330 (16)0.0072 (13)0.0024 (12)0.0048 (13)
C80.0303 (16)0.0371 (17)0.0293 (15)0.0026 (13)0.0010 (12)0.0014 (13)
C90.0285 (15)0.0310 (16)0.0390 (17)0.0039 (12)0.0038 (13)0.0077 (13)
C100.0265 (14)0.0309 (15)0.0329 (16)0.0029 (12)0.0024 (12)0.0053 (12)
C110.0255 (15)0.0358 (17)0.0382 (17)0.0015 (12)0.0028 (13)0.0112 (14)
C120.0271 (15)0.0357 (17)0.0428 (18)0.0020 (13)0.0026 (13)0.0091 (14)
C130.0330 (16)0.0370 (17)0.0390 (18)0.0014 (13)0.0028 (14)0.0143 (14)
C140.0287 (15)0.0362 (16)0.0269 (14)0.0041 (12)0.0016 (12)0.0080 (12)
C150.0251 (14)0.0329 (16)0.0302 (15)0.0013 (12)0.0010 (12)0.0066 (12)
C160.0317 (16)0.0353 (16)0.0269 (15)0.0059 (13)0.0019 (12)0.0074 (12)
C170.049 (2)0.045 (2)0.0304 (17)0.0088 (16)0.0089 (15)0.0065 (14)
C180.066 (3)0.059 (3)0.042 (2)0.013 (2)0.022 (2)0.0035 (19)
C190.066 (3)0.052 (2)0.053 (2)0.019 (2)0.013 (2)0.014 (2)
C200.0424 (19)0.0328 (17)0.048 (2)0.0073 (15)0.0021 (16)0.0064 (15)
C210.055 (2)0.0277 (17)0.067 (3)0.0118 (16)0.009 (2)0.0003 (17)
C220.111 (5)0.032 (2)0.122 (6)0.030 (3)0.015 (4)0.004 (3)
C230.116 (6)0.030 (2)0.141 (7)0.017 (3)0.015 (5)0.023 (3)
C240.059 (3)0.0320 (19)0.065 (3)0.0057 (17)0.010 (2)0.0135 (18)
C250.047 (2)0.0348 (18)0.049 (2)0.0035 (15)0.0007 (17)0.0165 (16)
C260.082 (4)0.060 (3)0.064 (3)0.004 (3)0.019 (3)0.038 (2)
C270.087 (4)0.072 (3)0.066 (3)0.013 (3)0.041 (3)0.028 (3)
C280.057 (2)0.052 (2)0.044 (2)0.0081 (19)0.0199 (19)0.0089 (18)
C290.0320 (16)0.0285 (15)0.0371 (17)0.0030 (12)0.0003 (13)0.0034 (13)
C300.0304 (15)0.0273 (15)0.0362 (16)0.0024 (12)0.0007 (13)0.0001 (12)
C310.049 (2)0.061 (3)0.040 (2)0.0011 (19)0.0132 (17)0.0023 (18)
C320.061 (3)0.084 (4)0.069 (3)0.006 (3)0.029 (3)0.027 (3)
C330.059 (3)0.065 (3)0.091 (4)0.016 (2)0.015 (3)0.035 (3)
C340.040 (2)0.038 (2)0.067 (3)0.0092 (16)0.0071 (18)0.0175 (18)
C350.052 (2)0.0293 (19)0.090 (4)0.0079 (17)0.025 (2)0.010 (2)
C360.108 (6)0.027 (2)0.164 (8)0.015 (3)0.047 (5)0.005 (4)
C370.122 (6)0.029 (2)0.147 (7)0.003 (3)0.037 (5)0.018 (3)
C380.061 (3)0.0285 (18)0.075 (3)0.0010 (17)0.023 (2)0.0097 (19)
C390.050 (2)0.0318 (18)0.050 (2)0.0046 (16)0.0110 (17)0.0113 (16)
C400.072 (3)0.055 (3)0.054 (3)0.014 (2)0.002 (2)0.025 (2)
C410.067 (3)0.067 (3)0.038 (2)0.008 (2)0.016 (2)0.009 (2)
C420.048 (2)0.046 (2)0.0312 (17)0.0009 (16)0.0083 (15)0.0050 (15)
C430.0330 (16)0.0294 (15)0.0342 (16)0.0000 (12)0.0047 (13)0.0035 (13)
C440.0308 (16)0.0288 (15)0.0373 (17)0.0026 (12)0.0027 (13)0.0042 (13)
N10.0336 (14)0.0295 (13)0.0307 (13)0.0040 (11)0.0041 (11)0.0008 (11)
N20.0370 (15)0.0308 (14)0.0368 (15)0.0023 (11)0.0073 (12)0.0021 (11)
N30.086 (3)0.041 (2)0.091 (3)0.028 (2)0.006 (3)0.010 (2)
N40.092 (3)0.039 (2)0.101 (4)0.010 (2)0.002 (3)0.032 (2)
N50.0356 (14)0.0360 (15)0.0300 (14)0.0032 (12)0.0029 (11)0.0006 (11)
N60.0370 (15)0.0312 (14)0.0273 (13)0.0026 (11)0.0025 (11)0.0014 (11)
N70.086 (3)0.040 (2)0.129 (5)0.022 (2)0.019 (3)0.023 (3)
N80.097 (4)0.034 (2)0.110 (4)0.008 (2)0.027 (3)0.025 (2)
O10.0341 (12)0.0315 (12)0.0504 (15)0.0095 (10)0.0017 (11)0.0017 (11)
O20.0493 (15)0.0424 (14)0.0387 (14)0.0153 (12)0.0084 (11)0.0117 (11)
O30.0348 (13)0.0447 (15)0.0699 (19)0.0169 (11)0.0047 (13)0.0188 (14)
O40.0324 (12)0.0468 (14)0.0371 (13)0.0101 (10)0.0058 (10)0.0080 (11)
O50.0378 (14)0.0566 (17)0.0409 (14)0.0113 (12)0.0061 (11)0.0168 (12)
O60.0342 (13)0.0321 (12)0.0549 (16)0.0020 (10)0.0019 (11)0.0042 (11)
O70.0449 (15)0.0430 (14)0.0442 (15)0.0060 (12)0.0050 (12)0.0161 (12)
O80.0294 (13)0.0476 (16)0.080 (2)0.0081 (11)0.0032 (13)0.0275 (15)
O90.0314 (12)0.0500 (15)0.0428 (14)0.0010 (11)0.0044 (10)0.0201 (12)
O100.0400 (14)0.0602 (17)0.0460 (15)0.0017 (12)0.0053 (11)0.0358 (13)
O1W0.0513 (16)0.0541 (17)0.0541 (17)0.0138 (13)0.0142 (13)0.0125 (14)
O2W0.0439 (15)0.0442 (15)0.0571 (17)0.0021 (12)0.0106 (13)0.0023 (13)
Geometric parameters (Å, º) top
Cd1—O72.205 (3)C21—C241.395 (7)
Cd1—O12.259 (2)C22—N31.331 (8)
Cd1—N22.339 (3)C22—C231.377 (11)
Cd1—O4i2.360 (2)C22—H22A0.9300
Cd1—N12.367 (3)C23—N41.326 (9)
Cd1—O5i2.384 (3)C23—H23A0.9300
Cd1—C8i2.711 (3)C24—N41.351 (6)
Cd2—O22.202 (2)C24—C251.457 (6)
Cd2—O62.295 (3)C25—C291.393 (5)
Cd2—N52.325 (3)C25—C261.402 (7)
Cd2—O9ii2.332 (2)C26—C271.369 (8)
Cd2—N62.343 (3)C26—H26A0.9300
Cd2—O10ii2.362 (3)C27—C281.396 (6)
Cd2—C16ii2.685 (3)C27—H27A0.9300
C1—O11.247 (4)C28—N21.323 (5)
C1—O21.271 (4)C28—H28A0.9300
C1—C21.497 (4)C29—N21.353 (4)
C2—C71.390 (4)C29—C301.459 (5)
C2—C31.392 (4)C30—N11.353 (4)
C3—C41.394 (4)C31—N51.325 (5)
C3—H3A0.9300C31—C321.397 (7)
C4—C51.391 (5)C31—H31A0.9300
C4—C81.499 (4)C32—C331.362 (9)
C5—C61.386 (5)C32—H32A0.9300
C5—H5A0.9300C33—C341.400 (8)
C6—O31.366 (4)C33—H33A0.9300
C6—C71.386 (5)C34—C441.408 (5)
C7—H7A0.9300C34—C351.447 (7)
C8—O51.245 (4)C35—N71.365 (6)
C8—O41.264 (4)C35—C381.396 (8)
C8—Cd1i2.711 (3)C36—N71.332 (10)
C9—O61.257 (4)C36—C371.389 (12)
C9—O71.272 (4)C36—H36A0.9300
C9—C101.485 (4)C37—N81.333 (9)
C10—C111.392 (4)C37—H37A0.9300
C10—C151.397 (4)C38—N81.346 (6)
C11—C121.392 (5)C38—C391.454 (6)
C11—H11A0.9300C39—C401.396 (7)
C12—O81.365 (4)C39—C431.400 (5)
C12—C131.383 (5)C40—C411.375 (7)
C13—C141.394 (5)C40—H40A0.9300
C13—H13A0.9300C41—C421.376 (6)
C14—C151.383 (4)C41—H41A0.9300
C14—C161.503 (4)C42—N61.335 (5)
C15—H15A0.9300C42—H42A0.9300
C16—O101.237 (4)C43—N61.348 (4)
C16—O91.266 (4)C43—C441.455 (5)
C16—Cd2ii2.685 (3)C44—N51.339 (5)
C17—N11.320 (5)O3—H3B0.8200
C17—C181.392 (6)O4—Cd1i2.360 (2)
C17—H17A0.9300O5—Cd1i2.384 (3)
C18—C191.372 (7)O8—H8A0.8200
C18—H18A0.9300O9—Cd2ii2.332 (2)
C19—C201.400 (6)O10—Cd2ii2.362 (3)
C19—H19A0.9300O1W—H1WA0.8500
C20—C301.396 (5)O1W—H1WB0.8500
C20—C211.457 (6)O2W—H2WA0.8500
C21—N31.354 (6)O2W—H2WB0.8499
O7—Cd1—O192.68 (10)C20—C19—H19A120.1
O7—Cd1—N2170.68 (10)C30—C20—C19117.5 (4)
O1—Cd1—N289.39 (10)C30—C20—C21119.9 (4)
O7—Cd1—O4i89.95 (10)C19—C20—C21122.5 (4)
O1—Cd1—O4i94.29 (9)N3—C21—C24122.4 (4)
N2—Cd1—O4i98.96 (10)N3—C21—C20117.7 (5)
O7—Cd1—N1101.48 (11)C24—C21—C20119.9 (4)
O1—Cd1—N1127.16 (9)N3—C22—C23122.1 (5)
N2—Cd1—N170.20 (10)N3—C22—H22A118.9
O4i—Cd1—N1135.72 (9)C23—C22—H22A118.9
O7—Cd1—O5i92.96 (11)N4—C23—C22123.9 (5)
O1—Cd1—O5i148.77 (9)N4—C23—H23A118.0
N2—Cd1—O5i89.96 (11)C22—C23—H23A118.0
O4i—Cd1—O5i55.03 (9)N4—C24—C21121.5 (4)
N1—Cd1—O5i81.52 (9)N4—C24—C25118.2 (5)
O7—Cd1—C8i90.03 (10)C21—C24—C25120.3 (4)
O1—Cd1—C8i122.03 (10)C29—C25—C26117.2 (4)
N2—Cd1—C8i96.58 (11)C29—C25—C24119.7 (4)
O4i—Cd1—C8i27.78 (9)C26—C25—C24123.0 (4)
N1—Cd1—C8i108.73 (10)C27—C26—C25119.7 (4)
O5i—Cd1—C8i27.34 (10)C27—C26—H26A120.1
O2—Cd2—O689.39 (10)C25—C26—H26A120.1
O2—Cd2—N5160.40 (10)C26—C27—C28119.4 (4)
O6—Cd2—N581.94 (10)C26—C27—H27A120.3
O2—Cd2—O9ii94.61 (10)C28—C27—H27A120.3
O6—Cd2—O9ii98.31 (9)N2—C28—C27121.9 (4)
N5—Cd2—O9ii103.99 (10)N2—C28—H28A119.1
O2—Cd2—N697.96 (11)C27—C28—H28A119.1
O6—Cd2—N6116.05 (10)N2—C29—C25122.7 (3)
N5—Cd2—N670.66 (10)N2—C29—C30117.1 (3)
O9ii—Cd2—N6143.34 (10)C25—C29—C30120.2 (3)
O2—Cd2—O10ii96.45 (11)N1—C30—C20122.3 (3)
O6—Cd2—O10ii153.41 (9)N1—C30—C29117.8 (3)
N5—Cd2—O10ii99.14 (11)C20—C30—C29119.9 (3)
O9ii—Cd2—O10ii55.45 (9)N5—C31—C32121.7 (5)
N6—Cd2—O10ii88.88 (9)N5—C31—H31A119.1
O2—Cd2—C16ii94.70 (10)C32—C31—H31A119.1
O6—Cd2—C16ii126.42 (10)C33—C32—C31119.5 (5)
N5—Cd2—C16ii104.61 (10)C33—C32—H32A120.3
O9ii—Cd2—C16ii28.12 (9)C31—C32—H32A120.3
N6—Cd2—C16ii116.16 (10)C32—C33—C34119.9 (4)
O10ii—Cd2—C16ii27.42 (9)C32—C33—H33A120.1
O1—C1—O2124.3 (3)C34—C33—H33A120.1
O1—C1—C2120.1 (3)C33—C34—C44117.0 (4)
O2—C1—C2115.6 (3)C33—C34—C35123.8 (4)
C7—C2—C3120.5 (3)C44—C34—C35119.1 (4)
C7—C2—C1119.4 (3)N7—C35—C38120.8 (5)
C3—C2—C1120.0 (3)N7—C35—C34118.1 (6)
C2—C3—C4119.2 (3)C38—C35—C34121.1 (4)
C2—C3—H3A120.4N7—C36—C37123.5 (6)
C4—C3—H3A120.4N7—C36—H36A118.3
C5—C4—C3120.1 (3)C37—C36—H36A118.3
C5—C4—C8119.4 (3)N8—C37—C36121.6 (6)
C3—C4—C8120.5 (3)N8—C37—H37A119.2
C6—C5—C4120.3 (3)C36—C37—H37A119.2
C6—C5—H5A119.9N8—C38—C35122.7 (5)
C4—C5—H5A119.9N8—C38—C39117.3 (5)
O3—C6—C5118.4 (3)C35—C38—C39120.0 (4)
O3—C6—C7121.6 (3)C40—C39—C43117.4 (4)
C5—C6—C7120.0 (3)C40—C39—C38123.2 (4)
C6—C7—C2119.9 (3)C43—C39—C38119.3 (4)
C6—C7—H7A120.0C41—C40—C39119.7 (4)
C2—C7—H7A120.0C41—C40—H40A120.2
O5—C8—O4121.7 (3)C39—C40—H40A120.2
O5—C8—C4119.4 (3)C40—C41—C42119.5 (4)
O4—C8—C4118.9 (3)C40—C41—H41A120.2
O5—C8—Cd1i61.56 (18)C42—C41—H41A120.2
O4—C8—Cd1i60.48 (17)N6—C42—C41121.9 (4)
C4—C8—Cd1i174.5 (3)N6—C42—H42A119.1
O6—C9—O7122.8 (3)C41—C42—H42A119.1
O6—C9—C10120.6 (3)N6—C43—C39122.0 (3)
O7—C9—C10116.6 (3)N6—C43—C44117.4 (3)
C11—C10—C15120.3 (3)C39—C43—C44120.6 (3)
C11—C10—C9118.7 (3)N5—C44—C34122.4 (4)
C15—C10—C9120.8 (3)N5—C44—C43117.7 (3)
C12—C11—C10120.0 (3)C34—C44—C43119.9 (4)
C12—C11—H11A120.0C17—N1—C30118.9 (3)
C10—C11—H11A120.0C17—N1—Cd1124.1 (2)
O8—C12—C13118.9 (3)C30—N1—Cd1115.3 (2)
O8—C12—C11121.4 (3)C28—N2—C29119.1 (3)
C13—C12—C11119.7 (3)C28—N2—Cd1123.2 (3)
C12—C13—C14120.2 (3)C29—N2—Cd1116.6 (2)
C12—C13—H13A119.9C22—N3—C21115.1 (6)
C14—C13—H13A119.9C23—N4—C24115.0 (6)
C15—C14—C13120.6 (3)C31—N5—C44119.5 (3)
C15—C14—C16120.3 (3)C31—N5—Cd2123.0 (3)
C13—C14—C16119.1 (3)C44—N5—Cd2117.4 (2)
C14—C15—C10119.1 (3)C42—N6—C43119.3 (3)
C14—C15—H15A120.4C42—N6—Cd2124.0 (2)
C10—C15—H15A120.4C43—N6—Cd2116.7 (2)
O10—C16—O9121.5 (3)C36—N7—C35115.4 (7)
O10—C16—C14119.6 (3)C37—N8—C38116.0 (7)
O9—C16—C14118.9 (3)C1—O1—Cd1139.9 (2)
O10—C16—Cd2ii61.58 (18)C1—O2—Cd2116.7 (2)
O9—C16—Cd2ii60.23 (17)C6—O3—H3B109.5
C14—C16—Cd2ii175.5 (2)C8—O4—Cd1i91.74 (19)
N1—C17—C18122.7 (4)C8—O5—Cd1i91.1 (2)
N1—C17—H17A118.6C9—O6—Cd2142.2 (2)
C18—C17—H17A118.6C9—O7—Cd1112.1 (2)
C19—C18—C17118.8 (4)C12—O8—H8A109.5
C19—C18—H18A120.6C16—O9—Cd2ii91.65 (19)
C17—C18—H18A120.6C16—O10—Cd2ii91.0 (2)
C18—C19—C20119.7 (4)H1WA—O1W—H1WB120.0
C18—C19—H19A120.1H2WA—O2W—H2WB120.0
O1—C1—C2—C7154.7 (3)O1—Cd1—N1—C17107.3 (3)
O2—C1—C2—C726.3 (5)N2—Cd1—N1—C17179.4 (3)
O1—C1—C2—C329.3 (5)O4i—Cd1—N1—C1797.0 (3)
O2—C1—C2—C3149.8 (3)O5i—Cd1—N1—C1786.3 (3)
C7—C2—C3—C42.3 (5)C8i—Cd1—N1—C1789.0 (3)
C1—C2—C3—C4173.8 (3)O7—Cd1—N1—C30169.8 (2)
C2—C3—C4—C52.6 (5)O1—Cd1—N1—C3087.8 (3)
C2—C3—C4—C8177.6 (3)N2—Cd1—N1—C3014.5 (2)
C3—C4—C5—C61.4 (5)O4i—Cd1—N1—C3067.9 (3)
C8—C4—C5—C6178.7 (3)O5i—Cd1—N1—C3078.5 (2)
C4—C5—C6—O3179.7 (3)C8i—Cd1—N1—C3075.8 (2)
C4—C5—C6—C70.1 (6)C27—C28—N2—C290.5 (7)
O3—C6—C7—C2179.9 (3)C27—C28—N2—Cd1168.1 (4)
C5—C6—C7—C20.5 (6)C25—C29—N2—C281.6 (5)
C3—C2—C7—C60.7 (5)C30—C29—N2—C28178.9 (3)
C1—C2—C7—C6175.3 (3)C25—C29—N2—Cd1166.8 (3)
C5—C4—C8—O517.3 (5)C30—C29—N2—Cd112.7 (4)
C3—C4—C8—O5162.5 (3)O7—Cd1—N2—C28150.5 (6)
C5—C4—C8—O4162.5 (3)O1—Cd1—N2—C2847.7 (3)
C3—C4—C8—O417.7 (5)O4i—Cd1—N2—C2846.6 (3)
C5—C4—C8—Cd1i116 (2)N1—Cd1—N2—C28177.9 (3)
C3—C4—C8—Cd1i64 (3)O5i—Cd1—N2—C28101.1 (3)
O6—C9—C10—C11156.7 (3)C8i—Cd1—N2—C2874.5 (3)
O7—C9—C10—C1124.2 (5)O7—Cd1—N2—C2941.6 (8)
O6—C9—C10—C1527.4 (5)O1—Cd1—N2—C29144.5 (3)
O7—C9—C10—C15151.7 (3)O4i—Cd1—N2—C29121.3 (2)
C15—C10—C11—C120.3 (5)N1—Cd1—N2—C2914.3 (2)
C9—C10—C11—C12175.6 (3)O5i—Cd1—N2—C2966.7 (2)
C10—C11—C12—O8178.8 (3)C8i—Cd1—N2—C2993.3 (3)
C10—C11—C12—C131.2 (6)C23—C22—N3—C210.8 (9)
O8—C12—C13—C14178.6 (3)C24—C21—N3—C221.6 (7)
C11—C12—C13—C141.0 (6)C20—C21—N3—C22179.9 (5)
C12—C13—C14—C150.7 (5)C22—C23—N4—C240.4 (10)
C12—C13—C14—C16180.0 (3)C21—C24—N4—C231.2 (8)
C13—C14—C15—C102.3 (5)C25—C24—N4—C23178.2 (5)
C16—C14—C15—C10178.5 (3)C32—C31—N5—C440.3 (6)
C11—C10—C15—C142.0 (5)C32—C31—N5—Cd2176.9 (4)
C9—C10—C15—C14173.8 (3)C34—C44—N5—C310.7 (5)
C15—C14—C16—O10162.0 (3)C43—C44—N5—C31179.3 (3)
C13—C14—C16—O1017.3 (5)C34—C44—N5—Cd2176.1 (3)
C15—C14—C16—O919.1 (5)C43—C44—N5—Cd24.0 (4)
C13—C14—C16—O9161.7 (3)O2—Cd2—N5—C31123.5 (4)
C15—C14—C16—Cd2ii58 (3)O6—Cd2—N5—C3159.0 (3)
C13—C14—C16—Cd2ii121 (3)O9ii—Cd2—N5—C3137.7 (3)
N1—C17—C18—C190.7 (7)N6—Cd2—N5—C31179.7 (3)
C17—C18—C19—C200.7 (7)O10ii—Cd2—N5—C3194.2 (3)
C18—C19—C20—C301.1 (7)C16ii—Cd2—N5—C3166.7 (3)
C18—C19—C20—C21178.4 (4)O2—Cd2—N5—C4453.1 (4)
C30—C20—C21—N3176.8 (4)O6—Cd2—N5—C44117.7 (3)
C19—C20—C21—N32.7 (6)O9ii—Cd2—N5—C44145.7 (2)
C30—C20—C21—C241.8 (6)N6—Cd2—N5—C443.6 (2)
C19—C20—C21—C24178.8 (4)O10ii—Cd2—N5—C4489.2 (2)
N3—C22—C23—N40.2 (12)C16ii—Cd2—N5—C44116.7 (2)
N3—C21—C24—N41.9 (7)C41—C42—N6—C430.3 (6)
C20—C21—C24—N4179.6 (4)C41—C42—N6—Cd2179.8 (3)
N3—C21—C24—C25177.5 (4)C39—C43—N6—C421.8 (5)
C20—C21—C24—C251.0 (6)C44—C43—N6—C42178.1 (3)
N4—C24—C25—C29179.1 (4)C39—C43—N6—Cd2178.0 (3)
C21—C24—C25—C290.3 (6)C44—C43—N6—Cd22.0 (4)
N4—C24—C25—C261.8 (7)O2—Cd2—N6—C4219.2 (3)
C21—C24—C25—C26178.8 (5)O6—Cd2—N6—C42112.5 (3)
C29—C25—C26—C270.6 (8)N5—Cd2—N6—C42177.2 (3)
C24—C25—C26—C27179.7 (5)O9ii—Cd2—N6—C4289.6 (3)
C25—C26—C27—C281.3 (9)O10ii—Cd2—N6—C4277.1 (3)
C26—C27—C28—N21.9 (9)C16ii—Cd2—N6—C4280.0 (3)
C26—C25—C29—N22.1 (6)O2—Cd2—N6—C43160.6 (2)
C24—C25—C29—N2178.8 (4)O6—Cd2—N6—C4367.4 (3)
C26—C25—C29—C30178.3 (4)N5—Cd2—N6—C432.9 (2)
C24—C25—C29—C300.8 (5)O9ii—Cd2—N6—C4390.5 (3)
C19—C20—C30—N10.3 (6)O10ii—Cd2—N6—C43103.0 (2)
C21—C20—C30—N1179.2 (3)C16ii—Cd2—N6—C43100.1 (2)
C19—C20—C30—C29179.2 (4)C37—C36—N7—C350.8 (10)
C21—C20—C30—C291.2 (5)C38—C35—N7—C361.9 (7)
N2—C29—C30—N10.9 (5)C34—C35—N7—C36178.5 (5)
C25—C29—C30—N1179.5 (3)C36—C37—N8—C381.4 (10)
N2—C29—C30—C20179.6 (3)C35—C38—N8—C370.3 (8)
C25—C29—C30—C200.0 (5)C39—C38—N8—C37179.4 (5)
N5—C31—C32—C331.1 (8)O2—C1—O1—Cd183.6 (5)
C31—C32—C33—C340.9 (8)C2—C1—O1—Cd195.4 (4)
C32—C33—C34—C440.1 (7)O7—Cd1—O1—C11.5 (4)
C32—C33—C34—C35179.0 (5)N2—Cd1—O1—C1169.4 (4)
C33—C34—C35—N72.4 (7)O4i—Cd1—O1—C191.7 (4)
C44—C34—C35—N7178.7 (4)N1—Cd1—O1—C1105.0 (4)
C33—C34—C35—C38177.9 (5)O5i—Cd1—O1—C1101.7 (4)
C44—C34—C35—C381.0 (6)C8i—Cd1—O1—C193.3 (4)
N7—C36—C37—N80.9 (12)O1—C1—O2—Cd27.4 (5)
N7—C35—C38—N81.4 (7)C2—C1—O2—Cd2171.6 (2)
C34—C35—C38—N8178.9 (4)O6—Cd2—O2—C161.2 (3)
N7—C35—C38—C39178.9 (4)N5—Cd2—O2—C12.2 (5)
C34—C35—C38—C390.8 (6)O9ii—Cd2—O2—C1159.5 (3)
N8—C38—C39—C401.0 (6)N6—Cd2—O2—C155.1 (3)
C35—C38—C39—C40178.8 (4)O10ii—Cd2—O2—C1144.8 (3)
N8—C38—C39—C43179.8 (4)C16ii—Cd2—O2—C1172.3 (3)
C35—C38—C39—C430.4 (6)O5—C8—O4—Cd1i6.4 (4)
C43—C39—C40—C410.3 (7)C4—C8—O4—Cd1i173.7 (3)
C38—C39—C40—C41179.5 (4)O4—C8—O5—Cd1i6.4 (4)
C39—C40—C41—C421.7 (7)C4—C8—O5—Cd1i173.8 (3)
C40—C41—C42—N62.1 (7)O7—C9—O6—Cd293.2 (5)
C40—C39—C43—N62.1 (5)C10—C9—O6—Cd285.9 (5)
C38—C39—C43—N6178.6 (3)O2—Cd2—O6—C910.2 (4)
C40—C39—C43—C44177.8 (4)N5—Cd2—O6—C9172.6 (4)
C38—C39—C43—C441.5 (5)O9ii—Cd2—O6—C984.4 (4)
C33—C34—C44—N50.9 (6)N6—Cd2—O6—C9108.8 (4)
C35—C34—C44—N5179.9 (3)O10ii—Cd2—O6—C993.1 (5)
C33—C34—C44—C43179.0 (4)C16ii—Cd2—O6—C985.2 (4)
C35—C34—C44—C430.1 (5)O6—C9—O7—Cd17.5 (4)
N6—C43—C44—N51.3 (5)C10—C9—O7—Cd1171.6 (2)
C39—C43—C44—N5178.6 (3)O1—Cd1—O7—C964.0 (3)
N6—C43—C44—C34178.8 (3)N2—Cd1—O7—C938.6 (8)
C39—C43—C44—C341.3 (5)O4i—Cd1—O7—C9158.3 (3)
C18—C17—N1—C301.5 (6)N1—Cd1—O7—C964.8 (3)
C18—C17—N1—Cd1165.9 (3)O5i—Cd1—O7—C9146.8 (3)
C20—C30—N1—C171.0 (5)C8i—Cd1—O7—C9174.0 (3)
C29—C30—N1—C17179.4 (3)O10—C16—O9—Cd2ii6.2 (4)
C20—C30—N1—Cd1166.7 (3)C14—C16—O9—Cd2ii174.9 (3)
C29—C30—N1—Cd113.8 (4)O9—C16—O10—Cd2ii6.1 (4)
O7—Cd1—N1—C175.0 (3)C14—C16—O10—Cd2ii175.0 (3)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3B···O2Wiii0.821.842.659 (4)177
O8—H8A···O1Wiv0.821.852.672 (4)177
O1W—H1WA···O9v0.852.142.912 (4)150
O1W—H1WB···O2v0.852.272.963 (4)138
O2W—H2WA···O4vi0.852.282.880 (4)127
O2W—H2WB···O7vi0.852.332.955 (4)131
Symmetry codes: (iii) x, y1, z; (iv) x1, y1, z; (v) x, y+1, z; (vi) x+1, y+1, z.

Experimental details

Crystal data
Chemical formula[Cd2(C8H4O5)2(C14H8N4)2]·2H2O
Mr1085.54
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)8.6754 (13), 15.1114 (17), 15.629 (3)
α, β, γ (°)92.903 (16), 97.143 (13), 95.515 (9)
V3)2019.6 (5)
Z2
Radiation typeMo Kα
µ (mm1)1.13
Crystal size (mm)0.37 × 0.33 × 0.27
Data collection
DiffractometerBruker APEX area-detector
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.681, 0.751
No. of measured, independent and
observed [I > 2σ(I)] reflections
11100, 9275, 8147
Rint0.061
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.031, 0.114, 1.07
No. of reflections9275
No. of parameters595
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.70, 1.43

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008).

Selected bond lengths (Å) top
Cd1—O72.205 (3)Cd2—O22.202 (2)
Cd1—O12.259 (2)Cd2—O62.295 (3)
Cd1—N22.339 (3)Cd2—N52.325 (3)
Cd1—O4i2.360 (2)Cd2—O9ii2.332 (2)
Cd1—N12.367 (3)Cd2—N62.343 (3)
Cd1—O5i2.384 (3)Cd2—O10ii2.362 (3)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3B···O2Wiii0.821.842.659 (4)176.8
O8—H8A···O1Wiv0.821.852.672 (4)177.4
O1W—H1WA···O9v0.852.142.912 (4)150.1
O1W—H1WB···O2v0.852.272.963 (4)138.2
O2W—H2WA···O4vi0.852.282.880 (4)127.4
O2W—H2WB···O7vi0.852.332.955 (4)130.5
Symmetry codes: (iii) x, y1, z; (iv) x1, y1, z; (v) x, y+1, z; (vi) x+1, y+1, z.
 

Acknowledgements

The author thanks the Program for the Foundation of Liaoning Province (L2010148) and phD Initial Funding Project of Liaoning Province (2010010174–401).

References

First citationBruker (2001). SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationHan, Z.-B., Ji, J.-W., An, H.-Y., Zhang, W., Han, G.-X., Zhang, G.-X. & Yang, L.-G. (2009). Dalton Trans. pp. 9807–9811.  Web of Science CSD CrossRef Google Scholar
First citationHe, Y.-K. & Han, Z.-B. (2006). Acta Cryst. E62, m2676–m2677.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationWang, X.-L., Bi, Y. F., Lin, H. Y. & Liu, G. C. (2007). Cryst. Growth Des. 72, 1086–1091.  Web of Science CSD CrossRef Google Scholar

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Volume 68| Part 4| April 2012| Pages m477-m478
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