A fivefold inter­penetrating diamondoid framework constructed by flexible dipyridyl and di­carboxyl­ate ligands

A novel three-dimensional Cd^II complex, poly[aqua­{[mu]₂-1,4-bis­[2-(pyridin-4-yl)ethenyl]benzene-[kappa]²N:N'}[[mu]₄-2,2'-(1,4-phenyl­ene)di­acetato-[kappa]⁴O,O':O'',O''']cadmium(II)], [Cd(C₁₀H₈O₄)(C₂₀H₁₆N₂)(H₂O)]_n, has been prepared by hydro­thermal assembly of Cd(NO₃)₂·4H₂O, 1,4-bis­[2-(pyridin-4-yl)ethenyl]benzene (1,4-bpeb) and 2,2'-(1,4-phenyl­ene)di­acetic acid (1,4-H₂pda). Each Cd^II centre is located on a twofold axis in a distorted penta­gonal bipyramidal coordination environment formed by one O atom from a water mol­ecule, which lies on the same twofold axis, four O atoms from two different 1,4-pda ligands and two N atoms from two different 1,4-bpeb ligands. The Cd^II centres are bridged by the 1,4-bpeb and 1,4-pda ligands, which lie across centres of inversion. The three-dimensional net can be regarded as a diamondoid network by treating the Cd^II atoms as nodes and the 1,4-bpeb and 1,4-pda ligands as linkers. The single net leaves voids that are filled by mutual inter­penetration of four independent equivalent frameworks in a fivefold inter­penetrating architecture.

Computing details

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).

Poly[aqua{µ₂-1,4-bis[2-(pyridin-4-yl)ethenyl]benzene-κ²N:N'}[µ₄-2,2'-(1,4-phenylene)diacetato-κ⁴O,O':O'',O''']cadmium(II)]

Crystal data

[Cd(C10H8O4)(C20H16N2)(H2O)]	F(000) = 1232
Mr = 606.94	Dx = 1.572 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 6132 reflections
a = 18.537 (4) Å	θ = 3.0–27.5°
b = 16.886 (3) Å	µ = 0.90 mm^−1
c = 8.3534 (17) Å	T = 223 K
β = 101.26 (3)°	Block, yellow
V = 2564.4 (9) Å^3	0.20 × 0.17 × 0.15 mm
Z = 4

Data collection

Bruker SMART CCD area-detector diffractometer	2937 independent reflections
Radiation source: fine-focus sealed tube	2641 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.033
φ and ω scans	θmax = 27.5°, θmin = 3.2°
Absorption correction: multi-scan (SADABS; Bruker, 1997)	h = −24→17
Tmin = 0.841, Tmax = 0.877	k = −20→21
11458 measured reflections	l = −10→9

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.032	H-atom parameters constrained
wR(F^2) = 0.077	w = 1/[σ^2(Fo^2) + (0.0429P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.14	(Δ/σ)max < 0.001
2937 reflections	Δρmax = 1.19 e Å^−3
174 parameters	Δρmin = −0.64 e Å^−3
0 restraints	Extinction correction: SHELXTL (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0073 (4)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Cd1	0.0000	0.371789 (12)	−0.2500	0.02882 (11)
N1	0.12006 (11)	0.38606 (11)	−0.0941 (2)	0.0344 (4)
O1	−0.04623 (11)	0.26880 (10)	−0.1026 (2)	0.0438 (4)
O2	−0.04436 (11)	0.38739 (10)	0.0024 (2)	0.0413 (4)
O3	0.0000	0.51095 (14)	−0.2500	0.0431 (6)
H1W	−0.0151	0.5424	−0.3289	0.065*
C1	0.17741 (14)	0.34306 (15)	−0.1179 (3)	0.0383 (5)
H1	0.1698	0.3046	−0.2010	0.046*
C2	0.24752 (14)	0.35233 (15)	−0.0264 (3)	0.0388 (5)
H2	0.2861	0.3205	−0.0482	0.047*
C3	0.26146 (13)	0.40866 (14)	0.0984 (3)	0.0348 (5)
C4	0.20107 (14)	0.45446 (14)	0.1198 (3)	0.0395 (6)
H4	0.2071	0.4942	0.2002	0.047*
C5	0.13303 (14)	0.44152 (14)	0.0238 (3)	0.0378 (5)
H5	0.0935	0.4730	0.0413	0.045*
C6	0.33442 (14)	0.41656 (15)	0.2006 (3)	0.0384 (5)
H6	0.3665	0.3731	0.2057	0.046*
C7	0.35898 (14)	0.48043 (15)	0.2871 (3)	0.0380 (5)
H7	0.3269	0.5240	0.2788	0.046*
C8	0.43147 (13)	0.48958 (14)	0.3944 (3)	0.0342 (5)
C9	0.45649 (14)	0.56443 (14)	0.4483 (3)	0.0371 (5)
H9	0.4267	0.6087	0.4141	0.045*
C10	0.47621 (14)	0.42438 (14)	0.4496 (3)	0.0374 (5)
H10	0.4604	0.3729	0.4170	0.045*
C11	−0.20096 (14)	0.18840 (15)	0.0389 (3)	0.0409 (6)
H11	−0.1679	0.1459	0.0644	0.049*
C12	−0.17611 (13)	0.26537 (15)	0.0695 (3)	0.0359 (5)
C13	−0.22592 (15)	0.32652 (15)	0.0292 (3)	0.0426 (6)
H13	−0.2099	0.3791	0.0483	0.051*
C14	−0.09549 (14)	0.28267 (17)	0.1395 (3)	0.0430 (6)
H14A	−0.0707	0.2340	0.1845	0.052*
H14B	−0.0917	0.3215	0.2279	0.052*
C15	−0.05847 (12)	0.31506 (14)	0.0051 (3)	0.0325 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd1	0.02084 (15)	0.02927 (16)	0.03468 (16)	0.000	0.00127 (9)	0.000
N1	0.0245 (11)	0.0354 (10)	0.0402 (10)	0.0001 (8)	−0.0010 (8)	0.0020 (8)
O1	0.0516 (12)	0.0328 (9)	0.0510 (10)	−0.0015 (8)	0.0198 (8)	0.0004 (7)
O2	0.0469 (11)	0.0355 (9)	0.0410 (9)	−0.0082 (8)	0.0069 (8)	−0.0027 (7)
O3	0.0539 (17)	0.0311 (12)	0.0397 (12)	0.000	−0.0025 (11)	0.000
C1	0.0313 (14)	0.0361 (12)	0.0438 (13)	0.0012 (10)	−0.0020 (10)	−0.0029 (10)
C2	0.0260 (13)	0.0395 (13)	0.0486 (14)	0.0043 (10)	0.0014 (10)	−0.0018 (10)
C3	0.0251 (12)	0.0355 (12)	0.0408 (12)	−0.0042 (10)	−0.0013 (9)	0.0030 (9)
C4	0.0320 (14)	0.0390 (13)	0.0443 (13)	0.0005 (10)	0.0000 (10)	−0.0059 (10)
C5	0.0279 (13)	0.0381 (13)	0.0449 (13)	0.0040 (10)	0.0012 (10)	−0.0012 (10)
C6	0.0240 (13)	0.0440 (14)	0.0447 (13)	−0.0002 (10)	0.0011 (10)	−0.0016 (10)
C7	0.0288 (13)	0.0390 (13)	0.0444 (13)	−0.0013 (10)	0.0028 (10)	0.0013 (10)
C8	0.0259 (13)	0.0377 (13)	0.0374 (11)	−0.0027 (10)	0.0024 (9)	−0.0012 (9)
C9	0.0300 (13)	0.0329 (12)	0.0456 (13)	0.0015 (10)	0.0006 (10)	0.0006 (9)
C10	0.0307 (14)	0.0330 (12)	0.0460 (13)	−0.0049 (10)	0.0012 (10)	−0.0033 (9)
C11	0.0355 (14)	0.0407 (13)	0.0465 (13)	0.0005 (11)	0.0082 (11)	0.0047 (10)
C12	0.0298 (13)	0.0481 (14)	0.0303 (11)	−0.0074 (10)	0.0075 (9)	0.0014 (9)
C13	0.0410 (15)	0.0361 (13)	0.0507 (14)	−0.0090 (11)	0.0091 (11)	−0.0013 (10)
C14	0.0332 (14)	0.0570 (16)	0.0380 (13)	−0.0088 (12)	0.0046 (10)	0.0055 (11)
C15	0.0193 (11)	0.0391 (13)	0.0364 (12)	−0.0022 (9)	−0.0013 (9)	0.0029 (9)

Geometric parameters (Å, º)

Cd1—O3	2.350 (2)	C5—H5	0.9400
Cd1—N1^i	2.361 (2)	C6—C7	1.328 (3)
Cd1—N1	2.361 (2)	C6—H6	0.9400
Cd1—O1	2.3845 (17)	C7—C8	1.471 (3)
Cd1—O1^i	2.3845 (17)	C7—H7	0.9400
Cd1—O2^i	2.4221 (18)	C8—C9	1.390 (3)
Cd1—O2	2.4221 (18)	C8—C10	1.401 (3)
Cd1—C15	2.745 (2)	C9—C10^ii	1.380 (3)
Cd1—C15^i	2.745 (2)	C9—H9	0.9400
N1—C1	1.334 (3)	C10—C9^ii	1.380 (3)
N1—C5	1.346 (3)	C10—H10	0.9400
O1—C15	1.246 (3)	C11—C12	1.386 (3)
O2—C15	1.250 (3)	C11—C13^iii	1.387 (4)
O3—H1W	0.8499	C11—H11	0.9400
C1—C2	1.382 (3)	C12—C13	1.382 (4)
C1—H1	0.9400	C12—C14	1.523 (3)
C2—C3	1.397 (3)	C13—C11^iii	1.387 (4)
C2—H2	0.9400	C13—H13	0.9400
C3—C4	1.401 (3)	C14—C15	1.526 (3)
C3—C6	1.458 (3)	C14—H14A	0.9800
C4—C5	1.374 (3)	C14—H14B	0.9800
C4—H4	0.9400
O3—Cd1—N1^i	84.15 (5)	C3—C2—H2	119.8
O3—Cd1—N1	84.14 (5)	C2—C3—C4	115.8 (2)
N1^i—Cd1—N1	168.29 (9)	C2—C3—C6	121.0 (2)
O3—Cd1—O1	136.83 (4)	C4—C3—C6	123.2 (2)
N1^i—Cd1—O1	87.94 (7)	C5—C4—C3	120.2 (2)
N1—Cd1—O1	100.65 (7)	C5—C4—H4	119.9
O3—Cd1—O1^i	136.83 (4)	C3—C4—H4	119.9
N1^i—Cd1—O1^i	100.64 (7)	N1—C5—C4	123.4 (2)
N1—Cd1—O1^i	87.94 (7)	N1—C5—H5	118.3
O1—Cd1—O1^i	86.35 (8)	C4—C5—H5	118.3
O3—Cd1—O2^i	83.75 (4)	C7—C6—C3	125.0 (2)
N1^i—Cd1—O2^i	87.28 (7)	C7—C6—H6	117.5
N1—Cd1—O2^i	91.45 (7)	C3—C6—H6	117.5
O1—Cd1—O2^i	138.24 (6)	C6—C7—C8	126.3 (2)
O1^i—Cd1—O2^i	54.03 (6)	C6—C7—H7	116.8
O3—Cd1—O2	83.76 (4)	C8—C7—H7	116.8
N1^i—Cd1—O2	91.45 (7)	C9—C8—C10	118.0 (2)
N1—Cd1—O2	87.28 (7)	C9—C8—C7	120.0 (2)
O1—Cd1—O2	54.03 (6)	C10—C8—C7	122.0 (2)
O1^i—Cd1—O2	138.24 (6)	C10^ii—C9—C8	121.9 (2)
O2^i—Cd1—O2	167.51 (8)	C10^ii—C9—H9	119.0
O3—Cd1—C15	110.42 (5)	C8—C9—H9	119.0
N1^i—Cd1—C15	89.50 (7)	C9^ii—C10—C8	120.1 (2)
N1—Cd1—C15	94.59 (7)	C9^ii—C10—H10	120.0
O1—Cd1—C15	26.95 (6)	C8—C10—H10	120.0
O1^i—Cd1—C15	112.49 (7)	C12—C11—C13^iii	120.6 (2)
O2^i—Cd1—C15	165.07 (7)	C12—C11—H11	119.7
O2—Cd1—C15	27.09 (6)	C13^iii—C11—H11	119.7
O3—Cd1—C15^i	110.42 (5)	C13—C12—C11	118.3 (2)
N1^i—Cd1—C15^i	94.59 (7)	C13—C12—C14	120.6 (2)
N1—Cd1—C15^i	89.50 (7)	C11—C12—C14	121.1 (2)
O1—Cd1—C15^i	112.49 (7)	C12—C13—C11^iii	121.1 (2)
O1^i—Cd1—C15^i	26.95 (6)	C12—C13—H13	119.4
O2^i—Cd1—C15^i	27.09 (6)	C11^iii—C13—H13	119.4
O2—Cd1—C15^i	165.07 (7)	C12—C14—C15	109.57 (19)
C15—Cd1—C15^i	139.16 (10)	C12—C14—H14A	109.8
C1—N1—C5	117.0 (2)	C15—C14—H14A	109.8
C1—N1—Cd1	123.71 (16)	C12—C14—H14B	109.8
C5—N1—Cd1	119.27 (16)	C15—C14—H14B	109.8
C15—O1—Cd1	92.89 (14)	H14A—C14—H14B	108.2
C15—O2—Cd1	91.02 (13)	O1—C15—O2	122.1 (2)
Cd1—O3—H1W	128.6	O1—C15—C14	118.6 (2)
N1—C1—C2	123.1 (2)	O2—C15—C14	119.3 (2)
N1—C1—H1	118.4	O1—C15—Cd1	60.16 (12)
C2—C1—H1	118.4	O2—C15—Cd1	61.90 (12)
C1—C2—C3	120.4 (2)	C14—C15—Cd1	176.42 (16)
C1—C2—H2	119.8

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