Poly[[tris­(1,10-phenanthroline)tris­(μ3-succinato)tricadmium(II)] tetra­hydrate]

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

doi:10.1107/S1600536807051665

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Poly[[tris(1,10-phenanthroline)tris(μ₃-succinato)tricadmium(II)] tetrahydrate]

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

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.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807051665/hg2314sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807051665/hg2314Isup2.hkl Contains datablock I

CCDC reference: 672582

checkCIF report

Key indicators

Single-crystal X-ray study
T = 298 K
Mean (C-C) = 0.004 Å
R factor = 0.035
wR factor = 0.073
Data-to-parameter ratio = 16.1

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.99
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O5
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O6
PLAT731_ALERT_1_C Bond    Calc     0.80(4), Rep   0.791(18) ......       2.22 su-Ra
              O7   -H7A     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.80(4), Rep   0.791(18) ......       2.22 su-Ra
              O7   -H7A     1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     2.17(4), Rep   2.174(19) ......       2.11 su-Ra
              H7A  -O8      1.555   5.666

Alert level G
PLAT794_ALERT_5_G Check Predicted Bond Valency for Cd1         (2)       2.05
PLAT794_ALERT_5_G Check Predicted Bond Valency for Cd2         (2)       2.00
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......          4

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   6 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

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.

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

	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]
	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]·4H₂O	F(000) = 2584
M_r = 1298.09	D_x = 1.811 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 6336 reflections
a = 11.1875 (6) Å	θ = 2.5–28.2°
b = 21.4051 (15) Å	µ = 1.41 mm⁻¹
c = 20.2455 (12) Å	T = 298 K
β = 100.847 (1)°	Block, colorless
V = 4761.6 (5) Å³	0.32 × 0.20 × 0.20 mm
Z = 4

Data collection top

Bruker SMART CCD area-detector diffractometer	5526 independent reflections
Radiation source: fine-focus sealed tube	4640 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.073
ϕ and ω scans	θ_max = 27.8°, θ_min = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −14→14
T_min = 0.662, T_max = 0.766	k = −22→27
16149 measured reflections	l = −18→26

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.035	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.073	w = 1/[σ²(F_o²) + (0.0314P)²] where P = (F_o² + 2F_c²)/3
S = 0.97	(Δ/σ)_max = 0.002
5526 reflections	Δρ_max = 0.74 e Å⁻³
343 parameters	Δρ_min = −0.79 e Å⁻³
4 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00223 (7)

Crystal data top

[Cd₃(C₄H₄O₄)₃(C₁₂H₈N₂)₃]·4H₂O	V = 4761.6 (5) Å³
M_r = 1298.09	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 11.1875 (6) Å	µ = 1.41 mm⁻¹
b = 21.4051 (15) Å	T = 298 K
c = 20.2455 (12) Å	0.32 × 0.20 × 0.20 mm
β = 100.847 (1)°

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)
T_min = 0.662, T_max = 0.766	R_int = 0.073
16149 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.035	4 restraints
wR(F²) = 0.073	H atoms treated by a mixture of independent and constrained refinement
S = 0.97	Δρ_max = 0.74 e Å⁻³
5526 reflections	Δρ_min = −0.79 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

	x	y	z	U_iso*/U_eq
Cd1	0.5000	0.450298 (13)	0.2500	0.03689 (9)
Cd2	0.785266 (16)	0.558555 (9)	0.372822 (9)	0.02702 (8)
N1	0.4185 (2)	0.36355 (11)	0.18944 (13)	0.0408 (6)
N2	0.73872 (19)	0.66078 (10)	0.33202 (11)	0.0320 (5)
N3	0.86461 (19)	0.63215 (11)	0.45773 (11)	0.0324 (5)
O1	0.63997 (18)	0.46118 (10)	0.18172 (10)	0.0470 (5)
O2	0.66807 (15)	0.51931 (9)	0.27212 (9)	0.0328 (4)
O3	1.0882 (2)	0.46530 (13)	0.15096 (13)	0.0661 (7)
O4	1.01226 (19)	0.56006 (11)	0.14051 (11)	0.0531 (6)
O5	0.59517 (19)	0.55649 (11)	0.41393 (12)	0.0566 (7)
O6	0.74168 (19)	0.49423 (10)	0.45879 (11)	0.0498 (5)
C1	0.7021 (2)	0.50054 (12)	0.21886 (13)	0.0296 (6)
C2	0.8143 (2)	0.52649 (13)	0.19883 (13)	0.0321 (6)
H2A	0.8672	0.5432	0.2384	0.038*
H2B	0.7914	0.5607	0.1676	0.038*
C3	0.8840 (2)	0.47844 (15)	0.16635 (17)	0.0467 (8)
H3A	0.9004	0.4426	0.1960	0.056*
H3B	0.8332	0.4644	0.1248	0.056*
C4	1.0029 (3)	0.50216 (17)	0.15113 (14)	0.0446 (8)
C5	0.3448 (3)	0.36281 (16)	0.13045 (17)	0.0515 (8)
H5	0.3145	0.4007	0.1121	0.062*
C6	0.3099 (3)	0.30888 (18)	0.09421 (18)	0.0598 (9)
H6	0.2596	0.3108	0.0521	0.072*
C7	0.3511 (3)	0.25281 (17)	0.12167 (18)	0.0571 (9)
H7	0.3290	0.2160	0.0982	0.069*
C8	0.4264 (3)	0.25086 (14)	0.18520 (16)	0.0423 (7)
C9	0.4599 (2)	0.30787 (13)	0.21748 (14)	0.0362 (6)
C10	0.4661 (3)	0.19347 (15)	0.21870 (16)	0.0549 (9)
H10	0.4449	0.1557	0.1970	0.066*
C11	0.6760 (3)	0.67523 (14)	0.27157 (14)	0.0408 (7)
H11	0.6429	0.6430	0.2431	0.049*
C12	0.6576 (3)	0.73636 (16)	0.24886 (15)	0.0491 (8)
H12	0.6125	0.7445	0.2063	0.059*
C13	0.7060 (3)	0.78405 (14)	0.28923 (16)	0.0468 (8)
H13	0.6956	0.8251	0.2741	0.056*
C14	0.7718 (2)	0.77134 (13)	0.35386 (14)	0.0367 (6)
C15	0.8255 (3)	0.81935 (14)	0.39966 (17)	0.0464 (7)
H15	0.8172	0.8610	0.3864	0.056*
C16	0.8867 (3)	0.80530 (15)	0.46072 (16)	0.0491 (8)
H16	0.9198	0.8373	0.4895	0.059*
C17	0.9027 (2)	0.74159 (14)	0.48317 (14)	0.0388 (7)
C18	0.9684 (3)	0.72468 (15)	0.54706 (15)	0.0475 (8)
H18	1.0030	0.7552	0.5774	0.057*
C19	0.9806 (3)	0.66304 (16)	0.56400 (15)	0.0483 (8)
H19	1.0238	0.6511	0.6059	0.058*
C20	0.9279 (3)	0.61835 (14)	0.51804 (14)	0.0402 (7)
H20	0.9375	0.5765	0.5302	0.048*
C21	0.8526 (2)	0.69322 (13)	0.43960 (12)	0.0308 (6)
C22	0.7853 (2)	0.70819 (13)	0.37350 (13)	0.0310 (6)
C23	0.6369 (3)	0.51558 (15)	0.45537 (15)	0.0413 (7)
C24	0.5619 (3)	0.48871 (19)	0.50365 (18)	0.0600 (10)
H24A	0.5593	0.4437	0.4983	0.072*
H24B	0.6037	0.4975	0.5492	0.072*
O7	0.3967 (2)	0.64187 (12)	0.38792 (14)	0.0622 (7)
H7A	0.345 (3)	0.630 (2)	0.407 (2)	0.093*
H7B	0.449 (3)	0.6154 (16)	0.393 (2)	0.093*
O8	0.8093 (2)	0.39279 (12)	0.54661 (12)	0.0548 (6)
H8A	0.870 (2)	0.4015 (19)	0.5751 (16)	0.082*
H8B	0.795 (4)	0.4228 (14)	0.5223 (18)	0.082*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.02758 (14)	0.02503 (16)	0.0631 (2)	0.000	0.02148 (13)	0.000
Cd2	0.02656 (11)	0.02609 (12)	0.03117 (12)	−0.00091 (7)	0.01250 (8)	−0.00017 (8)
N1	0.0353 (12)	0.0292 (13)	0.0587 (16)	−0.0019 (10)	0.0106 (11)	0.0041 (11)
N2	0.0343 (11)	0.0322 (13)	0.0310 (12)	0.0016 (10)	0.0103 (9)	0.0010 (10)
N3	0.0362 (12)	0.0311 (13)	0.0324 (12)	0.0007 (9)	0.0128 (10)	0.0015 (10)
O1	0.0385 (11)	0.0575 (14)	0.0496 (13)	−0.0221 (10)	0.0201 (10)	−0.0225 (11)
O2	0.0295 (9)	0.0364 (11)	0.0350 (10)	−0.0037 (8)	0.0127 (8)	−0.0059 (8)
O3	0.0409 (12)	0.0809 (19)	0.0837 (18)	−0.0104 (12)	0.0299 (12)	−0.0349 (15)
O4	0.0417 (12)	0.0665 (17)	0.0543 (14)	−0.0193 (11)	0.0172 (10)	0.0069 (12)
O5	0.0424 (12)	0.0763 (18)	0.0572 (14)	0.0027 (11)	0.0247 (11)	0.0284 (12)
O6	0.0500 (12)	0.0432 (13)	0.0642 (14)	0.0047 (10)	0.0316 (11)	0.0120 (11)
C1	0.0264 (12)	0.0305 (15)	0.0335 (14)	0.0007 (10)	0.0101 (11)	0.0031 (11)
C2	0.0320 (13)	0.0345 (15)	0.0319 (14)	−0.0093 (11)	0.0116 (11)	−0.0011 (11)
C3	0.0364 (15)	0.0452 (19)	0.064 (2)	−0.0122 (13)	0.0230 (15)	−0.0141 (16)
C4	0.0331 (15)	0.072 (2)	0.0319 (16)	−0.0175 (15)	0.0157 (12)	−0.0220 (15)
C5	0.0461 (18)	0.046 (2)	0.060 (2)	−0.0029 (15)	0.0047 (16)	0.0103 (16)
C6	0.055 (2)	0.065 (3)	0.056 (2)	−0.0097 (18)	0.0013 (17)	0.0028 (18)
C7	0.055 (2)	0.050 (2)	0.067 (2)	−0.0192 (17)	0.0125 (17)	−0.0137 (18)
C8	0.0390 (15)	0.0310 (16)	0.061 (2)	−0.0066 (12)	0.0186 (15)	−0.0038 (14)
C9	0.0298 (13)	0.0275 (15)	0.0547 (18)	−0.0018 (11)	0.0167 (12)	−0.0005 (12)
C10	0.061 (2)	0.0271 (16)	0.080 (3)	−0.0087 (14)	0.0217 (18)	−0.0086 (15)
C11	0.0446 (16)	0.0415 (18)	0.0365 (16)	0.0027 (13)	0.0082 (13)	−0.0006 (13)
C12	0.0499 (18)	0.058 (2)	0.0382 (17)	0.0103 (16)	0.0056 (14)	0.0115 (15)
C13	0.0520 (18)	0.0348 (17)	0.057 (2)	0.0097 (14)	0.0190 (16)	0.0129 (15)
C14	0.0374 (14)	0.0297 (15)	0.0468 (17)	0.0027 (12)	0.0172 (13)	0.0032 (12)
C15	0.0513 (18)	0.0258 (16)	0.063 (2)	−0.0011 (13)	0.0137 (16)	−0.0008 (14)
C16	0.0548 (18)	0.0301 (17)	0.061 (2)	−0.0092 (14)	0.0079 (16)	−0.0080 (15)
C17	0.0391 (15)	0.0344 (16)	0.0444 (17)	−0.0051 (12)	0.0118 (13)	−0.0064 (13)
C18	0.0512 (18)	0.048 (2)	0.0405 (18)	−0.0096 (15)	0.0005 (14)	−0.0127 (15)
C19	0.0488 (18)	0.058 (2)	0.0365 (17)	−0.0036 (16)	0.0026 (14)	0.0002 (15)
C20	0.0440 (16)	0.0386 (17)	0.0385 (16)	0.0026 (13)	0.0090 (13)	0.0035 (13)
C21	0.0305 (13)	0.0308 (15)	0.0341 (15)	−0.0005 (11)	0.0138 (11)	−0.0013 (11)
C22	0.0293 (13)	0.0297 (15)	0.0367 (15)	−0.0010 (11)	0.0129 (11)	−0.0001 (12)
C23	0.0432 (16)	0.0452 (18)	0.0407 (17)	−0.0085 (14)	0.0210 (13)	0.0028 (14)
C24	0.0496 (19)	0.076 (3)	0.062 (2)	0.0037 (18)	0.0282 (17)	0.0248 (19)
O7	0.0657 (17)	0.0497 (16)	0.0671 (17)	−0.0044 (13)	0.0022 (13)	0.0110 (13)
O8	0.0580 (14)	0.0522 (15)	0.0531 (16)	0.0038 (12)	0.0081 (11)	0.0067 (11)

Geometric parameters (Å, º) top

Cd1—O1ⁱ	2.2873 (19)	C6—C7	1.366 (5)
Cd1—O1	2.2873 (19)	C6—H6	0.9300
Cd1—N1	2.315 (2)	C7—C8	1.399 (4)
Cd1—N1ⁱ	2.315 (2)	C7—H7	0.9300
Cd1—O2	2.3667 (17)	C8—C9	1.402 (4)
Cd1—O2ⁱ	2.3667 (17)	C8—C10	1.433 (4)
Cd1—C1ⁱ	2.683 (2)	C9—C9ⁱ	1.447 (5)
Cd2—O4ⁱⁱ	2.331 (2)	C10—C10ⁱ	1.349 (6)
Cd2—O6	2.341 (2)	C10—H10	0.9300
Cd2—O2	2.3613 (17)	C11—C12	1.389 (4)
Cd2—N2	2.362 (2)	C11—H11	0.9300
Cd2—N3	2.377 (2)	C12—C13	1.355 (4)
Cd2—O5	2.426 (2)	C12—H12	0.9300
Cd2—O3ⁱⁱ	2.545 (3)	C13—C14	1.402 (4)
N1—C5	1.318 (4)	C13—H13	0.9300
N1—C9	1.363 (3)	C14—C22	1.409 (4)
N2—C11	1.328 (3)	C14—C15	1.438 (4)
N2—C22	1.357 (3)	C15—C16	1.330 (4)
N3—C20	1.324 (3)	C15—H15	0.9300
N3—C21	1.357 (4)	C16—C17	1.438 (4)
O1—C1	1.249 (3)	C16—H16	0.9300
O2—C1	1.274 (3)	C17—C21	1.407 (4)
O3—C4	1.239 (4)	C17—C18	1.409 (4)
O3—Cd2ⁱⁱ	2.545 (3)	C18—C19	1.364 (4)
O4—C4	1.265 (4)	C18—H18	0.9300
O4—Cd2ⁱⁱ	2.331 (2)	C19—C20	1.386 (4)
O5—C23	1.241 (4)	C19—H19	0.9300
O6—C23	1.248 (3)	C20—H20	0.9300
C1—C2	1.497 (3)	C21—C22	1.443 (3)
C2—C3	1.514 (4)	C23—C24	1.516 (4)
C2—H2A	0.9700	C24—C24ⁱⁱⁱ	1.448 (6)
C2—H2B	0.9700	C24—H24A	0.9700
C3—C4	1.509 (4)	C24—H24B	0.9700
C3—H3A	0.9700	O7—H7A	0.791 (18)
C3—H3B	0.9700	O7—H7B	0.804 (18)
C5—C6	1.384 (5)	O8—H8A	0.823 (18)
C5—H5	0.9300	O8—H8B	0.806 (19)

O1ⁱ—Cd1—O1	168.31 (11)	C4—C3—H3B	108.8
O1ⁱ—Cd1—N1	98.96 (9)	C2—C3—H3B	108.8
O1—Cd1—N1	90.44 (8)	H3A—C3—H3B	107.7
O1ⁱ—Cd1—N1ⁱ	90.44 (8)	O3—C4—O4	122.3 (3)
O1—Cd1—N1ⁱ	98.96 (9)	O3—C4—C3	119.7 (3)
N1—Cd1—N1ⁱ	73.37 (12)	O4—C4—C3	117.9 (3)
O1ⁱ—Cd1—O2	115.59 (7)	N1—C5—C6	123.8 (3)
O1—Cd1—O2	56.00 (6)	N1—C5—H5	118.1
N1—Cd1—O2	145.11 (7)	C6—C5—H5	118.1
N1ⁱ—Cd1—O2	100.42 (7)	C7—C6—C5	118.5 (3)
O1ⁱ—Cd1—O2ⁱ	56.00 (6)	C7—C6—H6	120.7
O1—Cd1—O2ⁱ	115.59 (7)	C5—C6—H6	120.7
N1—Cd1—O2ⁱ	100.42 (7)	C6—C7—C8	119.9 (3)
N1ⁱ—Cd1—O2ⁱ	145.11 (7)	C6—C7—H7	120.0
O2—Cd1—O2ⁱ	102.76 (9)	C8—C7—H7	120.0
O1ⁱ—Cd1—C1ⁱ	27.67 (7)	C7—C8—C9	117.7 (3)
O1—Cd1—C1ⁱ	143.51 (8)	C7—C8—C10	122.7 (3)
N1—Cd1—C1ⁱ	100.42 (8)	C9—C8—C10	119.6 (3)
N1ⁱ—Cd1—C1ⁱ	117.52 (8)	N1—C9—C8	121.8 (3)
O2—Cd1—C1ⁱ	112.32 (7)	N1—C9—C9ⁱ	118.86 (16)
O2ⁱ—Cd1—C1ⁱ	28.34 (7)	C8—C9—C9ⁱ	119.32 (18)
O4ⁱⁱ—Cd2—O6	115.91 (8)	C10ⁱ—C10—C8	120.94 (18)
O4ⁱⁱ—Cd2—O2	107.38 (7)	C10ⁱ—C10—H10	119.5
O6—Cd2—O2	105.85 (7)	C8—C10—H10	119.5
O4ⁱⁱ—Cd2—N2	95.84 (8)	N2—C11—C12	123.0 (3)
O6—Cd2—N2	137.87 (7)	N2—C11—H11	118.5
O2—Cd2—N2	88.71 (7)	C12—C11—H11	118.5
O4ⁱⁱ—Cd2—N3	80.55 (7)	C13—C12—C11	119.5 (3)
O6—Cd2—N3	87.36 (8)	C13—C12—H12	120.3
O2—Cd2—N3	158.64 (7)	C11—C12—H12	120.3
N2—Cd2—N3	70.53 (7)	C12—C13—C14	119.8 (3)
O4ⁱⁱ—Cd2—O5	166.83 (8)	C12—C13—H13	120.1
O6—Cd2—O5	54.24 (7)	C14—C13—H13	120.1
O2—Cd2—O5	84.81 (7)	C13—C14—C22	117.3 (3)
N2—Cd2—O5	89.26 (7)	C13—C14—C15	123.1 (3)
N3—Cd2—O5	89.78 (8)	C22—C14—C15	119.6 (3)
O4ⁱⁱ—Cd2—O3ⁱⁱ	53.26 (7)	C16—C15—C14	121.2 (3)
O6—Cd2—O3ⁱⁱ	83.13 (7)	C16—C15—H15	119.4
O2—Cd2—O3ⁱⁱ	78.21 (8)	C14—C15—H15	119.4
N2—Cd2—O3ⁱⁱ	138.96 (7)	C15—C16—C17	121.3 (3)
N3—Cd2—O3ⁱⁱ	120.76 (8)	C15—C16—H16	119.3
O5—Cd2—O3ⁱⁱ	127.25 (8)	C17—C16—H16	119.3
C5—N1—C9	118.2 (3)	C21—C17—C18	117.6 (3)
C5—N1—Cd1	127.3 (2)	C21—C17—C16	119.2 (3)
C9—N1—Cd1	114.31 (19)	C18—C17—C16	123.1 (3)
C11—N2—C22	118.1 (2)	C19—C18—C17	119.3 (3)
C11—N2—Cd2	125.57 (19)	C19—C18—H18	120.3
C22—N2—Cd2	116.27 (17)	C17—C18—H18	120.3
C20—N3—C21	118.2 (2)	C18—C19—C20	119.3 (3)
C20—N3—Cd2	125.52 (19)	C18—C19—H19	120.4
C21—N3—Cd2	115.99 (17)	C20—C19—H19	120.4
C1—O1—Cd1	94.09 (16)	N3—C20—C19	123.4 (3)
C1—O2—Cd2	129.59 (15)	N3—C20—H20	118.3
C1—O2—Cd1	89.78 (15)	C19—C20—H20	118.3
Cd2—O2—Cd1	132.66 (8)	N3—C21—C17	122.1 (2)
C4—O3—Cd2ⁱⁱ	87.5 (2)	N3—C21—C22	118.2 (2)
C4—O4—Cd2ⁱⁱ	96.86 (18)	C17—C21—C22	119.7 (3)
C23—O5—Cd2	90.14 (17)	N2—C22—C14	122.3 (2)
C23—O6—Cd2	93.92 (18)	N2—C22—C21	118.7 (2)
O1—C1—O2	120.1 (2)	C14—C22—C21	119.0 (2)
O1—C1—C2	119.1 (2)	O5—C23—O6	121.7 (3)
O2—C1—C2	120.8 (2)	O5—C23—C24	121.3 (3)
C1—C2—C3	113.1 (2)	O6—C23—C24	117.0 (3)
C1—C2—H2A	109.0	C24ⁱⁱⁱ—C24—C23	116.3 (4)
C3—C2—H2A	109.0	C24ⁱⁱⁱ—C24—H24A	108.2
C1—C2—H2B	109.0	C23—C24—H24A	108.2
C3—C2—H2B	109.0	C24ⁱⁱⁱ—C24—H24B	108.2
H2A—C2—H2B	107.8	C23—C24—H24B	108.2
C4—C3—C2	114.0 (3)	H24A—C24—H24B	107.4
C4—C3—H3A	108.8	H7A—O7—H7B	107 (4)
C2—C3—H3A	108.8	H8A—O8—H8B	107 (4)

O1ⁱ—Cd1—N1—C5	95.2 (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—C2	179.6 (2)
O2ⁱ—Cd1—N1—C5	38.4 (3)	Cd2—O2—C1—O1	153.3 (2)
C1ⁱ—Cd1—N1—C5	67.2 (3)	Cd1—O2—C1—O1	2.1 (3)
O1ⁱ—Cd1—N1—C9	−89.39 (19)	Cd2—O2—C1—C2	−28.5 (3)
O1—Cd1—N1—C9	97.6 (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—C9	82.7 (2)	O2—C1—C2—C3	144.2 (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—O4	0.8 (3)
O4ⁱⁱ—Cd2—N2—C11	103.4 (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—C3	177.4 (2)
N3—Cd2—N2—C11	−178.8 (2)	C2—C3—C4—O3	150.8 (3)
O5—Cd2—N2—C11	−88.8 (2)	C2—C3—C4—O4	−27.5 (4)
O3ⁱⁱ—Cd2—N2—C11	66.3 (3)	C9—N1—C5—C6	−2.2 (5)
O4ⁱⁱ—Cd2—N2—C22	−73.61 (18)	Cd1—N1—C5—C6	173.0 (3)
O6—Cd2—N2—C22	66.6 (2)	N1—C5—C6—C7	2.0 (5)
O2—Cd2—N2—C22	179.05 (18)	C5—C6—C7—C8	0.2 (5)
N3—Cd2—N2—C22	4.20 (17)	C6—C7—C8—C9	−1.9 (5)
O5—Cd2—N2—C22	94.23 (18)	C6—C7—C8—C10	175.8 (3)
O3ⁱⁱ—Cd2—N2—C22	−110.64 (19)	C5—N1—C9—C8	0.3 (4)
O4ⁱⁱ—Cd2—N3—C20	−78.7 (2)	Cd1—N1—C9—C8	−175.6 (2)
O6—Cd2—N3—C20	38.1 (2)	C5—N1—C9—C9ⁱ	−179.5 (3)
O2—Cd2—N3—C20	167.36 (19)	Cd1—N1—C9—C9ⁱ	4.7 (4)
N2—Cd2—N3—C20	−178.4 (2)	C7—C8—C9—N1	1.7 (4)
O5—Cd2—N3—C20	92.3 (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—C21	94.91 (18)	C10—C8—C9—C9ⁱ	3.7 (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—C10ⁱ	0.9 (6)
N2—Cd2—N3—C21	−4.78 (17)	C22—N2—C11—C12	0.9 (4)
O5—Cd2—N3—C21	−94.07 (18)	Cd2—N2—C11—C12	−176.0 (2)
O3ⁱⁱ—Cd2—N3—C21	131.33 (17)	N2—C11—C12—C13	0.6 (5)
O1ⁱ—Cd1—O1—C1	47.76 (16)	C11—C12—C13—C14	−1.3 (5)
N1—Cd1—O1—C1	−168.60 (18)	C12—C13—C14—C22	0.6 (4)
N1ⁱ—Cd1—O1—C1	−95.37 (18)	C12—C13—C14—C15	−179.8 (3)
O2—Cd1—O1—C1	1.21 (15)	C13—C14—C15—C16	179.7 (3)
O2ⁱ—Cd1—O1—C1	89.62 (17)	C22—C14—C15—C16	−0.8 (5)
C1ⁱ—Cd1—O1—C1	83.1 (2)	C14—C15—C16—C17	0.6 (5)
O4ⁱⁱ—Cd2—O2—C1	1.1 (2)	C15—C16—C17—C21	0.0 (5)
O6—Cd2—O2—C1	−123.3 (2)	C15—C16—C17—C18	179.1 (3)
N2—Cd2—O2—C1	96.8 (2)	C21—C17—C18—C19	0.0 (4)
N3—Cd2—O2—C1	110.3 (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—C19	1.2 (4)
O4ⁱⁱ—Cd2—O2—Cd1	140.17 (11)	Cd2—N3—C20—C19	174.7 (2)
O6—Cd2—O2—Cd1	15.78 (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—C22	179.1 (2)
O3ⁱⁱ—Cd2—O2—Cd1	95.05 (12)	Cd2—N3—C21—C22	5.0 (3)
O1ⁱ—Cd1—O2—C1	−171.79 (14)	C18—C17—C21—N3	0.9 (4)
O1—Cd1—O2—C1	−1.18 (15)	C16—C17—C21—N3	180.0 (3)
N1—Cd1—O2—C1	16.8 (2)	C18—C17—C21—C22	−179.6 (2)
N1ⁱ—Cd1—O2—C1	92.65 (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—C14	175.58 (19)
O1ⁱ—Cd1—O2—Cd2	38.54 (13)	C11—N2—C22—C21	179.4 (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—N2	0.9 (4)
N1ⁱ—Cd1—O2—Cd2	−57.02 (12)	C15—C14—C22—N2	−178.7 (2)
O2ⁱ—Cd1—O2—Cd2	96.72 (11)	C13—C14—C22—C21	179.8 (2)
C1ⁱ—Cd1—O2—Cd2	68.67 (12)	C15—C14—C22—C21	0.2 (4)
O4ⁱⁱ—Cd2—O5—C23	−43.9 (5)	N3—C21—C22—N2	−1.1 (3)
O6—Cd2—O5—C23	0.51 (18)	C17—C21—C22—N2	179.4 (2)
O2—Cd2—O5—C23	114.3 (2)	N3—C21—C22—C14	179.9 (2)
N2—Cd2—O5—C23	−156.9 (2)	C17—C21—C22—C14	0.4 (4)
N3—Cd2—O5—C23	−86.4 (2)	Cd2—O5—C23—O6	−0.9 (3)
O3ⁱⁱ—Cd2—O5—C23	43.4 (2)	Cd2—O5—C23—C24	179.8 (3)
O4ⁱⁱ—Cd2—O6—C23	169.29 (18)	Cd2—O6—C23—O5	0.9 (3)
O2—Cd2—O6—C23	−71.82 (19)	Cd2—O6—C23—C24	−179.8 (3)
N2—Cd2—O6—C23	34.4 (2)	O5—C23—C24—C24ⁱⁱⁱ	2.8 (6)
N3—Cd2—O6—C23	91.13 (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, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O8ⁱⁱⁱ	0.79 (2)	2.17 (2)	2.962 (4)	174 (5)
O7—H7B···O5	0.80 (2)	2.05 (2)	2.847 (3)	172 (4)
O8—H8A···O4^iv	0.82 (2)	2.04 (2)	2.857 (3)	169 (4)
O8—H8B···O6	0.81 (2)	2.02 (2)	2.818 (3)	174 (4)

Symmetry codes: (iii) −x+1, −y+1, −z+1; (iv) x, −y+1, z+1/2.

Experimental details

Crystal data
Chemical formula	[Cd₃(C₄H₄O₄)₃(C₁₂H₈N₂)₃]·4H₂O
M_r	1298.09
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	298
a, b, c (Å)	11.1875 (6), 21.4051 (15), 20.2455 (12)
β (°)	100.847 (1)
V (Å³)	4761.6 (5)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.41
Crystal size (mm)	0.32 × 0.20 × 0.20

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.662, 0.766
No. of measured, independent and observed [I > 2σ(I)] reflections	16149, 5526, 4640
R_int	0.073
(sin θ/λ)_max (Å⁻¹)	0.655

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.035, 0.073, 0.97
No. of reflections	5526
No. of parameters	343
No. of restraints	4
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.74, −0.79

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), SHELXTL (Bruker, 1997).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O8ⁱ	0.791 (18)	2.174 (19)	2.962 (4)	174 (5)
O7—H7B···O5	0.804 (18)	2.048 (19)	2.847 (3)	172 (4)
O8—H8A···O4ⁱⁱ	0.823 (18)	2.04 (2)	2.857 (3)	169 (4)
O8—H8B···O6	0.806 (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.

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