trans-Tetra-aqua-bis(nicotinamide-κN)cadmium(II) biphenyl-4,4'-disulfonate.

In the title compound, [Cd(C(6)H(6)N(2)O)(2)(H(2)O)(4)](C(10)H(8)O(6)S(2)), the Cd(II) ion is located on a crystallographic inversion centre. An octa-hedral coordination geometry is defined by four water mol-ecules in one plane, and two trans N-atom donors of the nicotinamide ligands. The biphenyl-4,4'-disulfonate anion also lies on a crystallographic inversion centre. In the crystal structure, the complex cations are connected to the counter-anions via N-H⋯O and O-H⋯O hydrogen bonds, forming a three-dimensional network.

Related literature

For related literature, see: Beatty (2001 ▶); Christer et al. (2004 ▶); Holman et al. (2001 ▶); Lian & Li (2007a ▶,b ▶,c ▶,d ▶).

Experimental

Crystal data

[Cd(C6H6N2O)2(H2O)4](C10H8O6S2)

M = 741.02

Monoclinic,

a = 14.742 (8) Å

b = 6.899 (4) Å

c = 15.292 (8) Å

β = 110.980 (9)°

V = 1452.2 (13) Å3

Z = 2

Mo Kα radiation

μ = 0.96 mm−1

T = 298 (2) K

0.40 × 0.36 × 0.31 mm

Data collection

Bruker SMART APEX CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.682, T max = 0.741

7656 measured reflections

2842 independent reflections

2477 reflections with I > 2σ(I)

R int = 0.034

Refinement

R[F 2 > 2σ(F 2)] = 0.030

wR(F 2) = 0.092

S = 1.07

2842 reflections

197 parameters

H-atom parameters constrained

Δρmax = 0.57 e Å−3

Δρmin = −1.19 e Å−3

Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808002390/fj2097sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808002390/fj2097Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Cd(C6H6N2O)2(H2O)4](C10H8O6S2)	F000 = 752
Mr = 741.02	Dx = 1.695 Mg m−3
Monoclinic, P2/c	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2yc	Cell parameters from 7656 reflections
a = 14.742 (8) Å	θ = 12–18º
b = 6.899 (4) Å	µ = 0.97 mm−1
c = 15.292 (8) Å	T = 298 (2) K
β = 110.980 (9)º	Block, colourless
V = 1452.2 (13) Å3	0.40 × 0.36 × 0.31 mm
Z = 2

Bruker SMART APEX CCD diffractometer	2842 independent reflections
Radiation source: fine-focus sealed tube	2477 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.034
T = 298(2) K	θmax = 26.0º
φ and ω scans	θmin = 3.3º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)	h = −18→12
Tmin = 0.682, Tmax = 0.741	k = −8→7
7656 measured reflections	l = −13→18

Refinement on F2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.030	w = 1/[σ2(Fo2) + (0.0578P)2 + 0.3728P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.092	(Δ/σ)max < 0.001
S = 1.07	Δρmax = 0.58 e Å−3
2842 reflections	Δρmin = −1.19 e Å−3
197 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.052 (2)
Secondary atom site location: difference Fourier map

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.

	x	y	z	Uiso*/Ueq
Cd1	0.5000	0.0000	0.5000	0.02772 (14)
S1	0.31842 (5)	0.50038 (6)	0.18505 (5)	0.03230 (18)
O1	0.03394 (9)	0.0836 (3)	0.40310 (11)	0.0485 (4)
O2	0.30985 (11)	0.3259 (3)	0.12698 (14)	0.0544 (5)
O3	0.39387 (14)	0.4851 (2)	0.27876 (16)	0.0462 (5)
O4	0.32299 (12)	0.6768 (3)	0.13379 (15)	0.0582 (5)
O5	0.51977 (12)	−0.2553 (3)	0.41016 (16)	0.0738 (7)
H5A	0.4803	−0.3193	0.3698	0.089*
H5B	0.5698	−0.2876	0.3976	0.089*
O6	0.51991 (12)	0.2033 (3)	0.38506 (14)	0.0657 (6)
H6A	0.4802	0.2889	0.3531	0.079*
H6B	0.5701	0.2527	0.3817	0.079*
N1	0.34204 (14)	−0.00860 (19)	0.41343 (14)	0.0296 (4)
N2	0.12317 (10)	−0.1123 (3)	0.52234 (10)	0.0370 (4)
H2A	0.0802	−0.1148	0.5484	0.044*
H2B	0.1766	−0.1754	0.5469	0.044*
C1	0.27511 (17)	−0.0072 (2)	0.45320 (16)	0.0279 (5)
H1	0.2932	−0.0044	0.5180	0.033*
C2	0.18103 (17)	−0.0100 (2)	0.39791 (17)	0.0277 (5)
C3	0.15424 (17)	−0.0111 (2)	0.29767 (16)	0.0316 (5)
H3	0.0888	−0.0066	0.2600	0.038*
C4	0.22217 (18)	−0.0186 (3)	0.25694 (16)	0.0334 (5)
H4	0.2057	−0.0249	0.1923	0.040*
C5	0.31554 (17)	−0.0164 (2)	0.31683 (16)	0.0320 (5)
H5	0.3645	−0.0202	0.2919	0.038*
C6	0.10639 (16)	−0.0082 (2)	0.44191 (16)	0.0302 (5)
C7	0.21328 (17)	0.5140 (2)	0.20881 (19)	0.0303 (5)
C8	0.21293 (18)	0.4744 (3)	0.30073 (19)	0.0348 (5)
H8	0.2707	0.4455	0.3494	0.042*
C9	0.12884 (18)	0.4791 (3)	0.31652 (19)	0.0349 (5)
H9	0.1271	0.4538	0.3756	0.042*
C10	0.04503 (16)	0.5228 (2)	0.24163 (18)	0.0311 (5)
C11	0.04791 (14)	0.5662 (3)	0.15037 (15)	0.0353 (4)
H11	−0.0095	0.5976	0.1017	0.042*
C12	0.13142 (14)	0.5621 (3)	0.13407 (14)	0.0342 (4)
H12	0.1338	0.5904	0.0754	0.041*

	U11	U22	U33	U12	U13	U23
Cd1	0.01281 (17)	0.03481 (19)	0.03689 (19)	−0.00051 (5)	0.01054 (11)	−0.00146 (6)
S1	0.0174 (3)	0.0352 (3)	0.0500 (4)	−0.00152 (14)	0.0190 (3)	−0.00351 (17)
O1	0.0210 (7)	0.0697 (11)	0.0582 (9)	0.0136 (8)	0.0181 (6)	0.0197 (9)
O2	0.0275 (8)	0.0627 (11)	0.0810 (11)	−0.0076 (8)	0.0290 (8)	−0.0316 (10)
O3	0.0196 (9)	0.0565 (11)	0.0619 (12)	−0.0001 (5)	0.0136 (8)	−0.0056 (6)
O4	0.0369 (9)	0.0594 (11)	0.0942 (13)	0.0054 (8)	0.0427 (9)	0.0243 (10)
O5	0.0318 (8)	0.0794 (13)	0.1183 (16)	−0.0128 (9)	0.0366 (10)	−0.0596 (13)
O6	0.0289 (8)	0.0791 (13)	0.0921 (13)	0.0042 (8)	0.0254 (8)	0.0459 (11)
N1	0.0152 (9)	0.0393 (10)	0.0338 (9)	−0.0004 (5)	0.0083 (7)	−0.0008 (6)
N2	0.0186 (7)	0.0542 (11)	0.0399 (9)	0.0035 (7)	0.0125 (6)	0.0069 (8)
C1	0.0161 (11)	0.0381 (12)	0.0295 (10)	−0.0004 (6)	0.0082 (8)	0.0001 (6)
C2	0.0189 (11)	0.0288 (10)	0.0353 (12)	0.0000 (6)	0.0095 (9)	−0.0004 (6)
C3	0.0184 (11)	0.0377 (12)	0.0340 (12)	0.0001 (6)	0.0036 (9)	0.0009 (7)
C4	0.0283 (12)	0.0421 (12)	0.0277 (10)	−0.0005 (7)	0.0075 (9)	−0.0006 (7)
C5	0.0228 (11)	0.0398 (11)	0.0362 (11)	0.0007 (7)	0.0139 (9)	−0.0008 (7)
C6	0.0154 (10)	0.0387 (12)	0.0352 (11)	−0.0019 (6)	0.0074 (8)	−0.0013 (7)
C7	0.0183 (11)	0.0288 (10)	0.0499 (13)	−0.0005 (6)	0.0197 (10)	−0.0014 (7)
C8	0.0212 (10)	0.0388 (10)	0.0483 (13)	0.0048 (7)	0.0172 (9)	0.0074 (8)
C9	0.0254 (11)	0.0388 (11)	0.0469 (12)	0.0054 (7)	0.0209 (10)	0.0098 (8)
C10	0.0200 (11)	0.0287 (9)	0.0508 (12)	0.0002 (7)	0.0202 (9)	−0.0007 (8)
C11	0.0195 (9)	0.0427 (11)	0.0454 (11)	0.0000 (9)	0.0139 (8)	−0.0004 (10)
C12	0.0237 (9)	0.0419 (10)	0.0412 (10)	−0.0029 (9)	0.0169 (8)	−0.0012 (10)

Cd1—N1i	2.230 (2)	C1—C2	1.341 (3)
Cd1—N1	2.230 (2)	C1—H1	0.9300
Cd1—O5i	2.316 (2)	C2—C3	1.439 (3)
Cd1—O5	2.316 (2)	C2—C6	1.481 (3)
Cd1—O6i	2.3479 (19)	C3—C4	1.357 (4)
Cd1—O6	2.3479 (19)	C3—H3	0.9300
S1—O4	1.463 (2)	C4—C5	1.353 (3)
S1—O3	1.470 (2)	C4—H4	0.9300
S1—O2	1.4742 (19)	C5—H5	0.9300
S1—C7	1.717 (2)	C7—C12	1.373 (3)
O1—C6	1.200 (3)	C7—C8	1.434 (4)
O5—H5A	0.8108	C8—C9	1.346 (3)
O5—H5B	0.8551	C8—H8	0.9300
O6—H6A	0.8517	C9—C10	1.384 (4)
O6—H6B	0.8328	C9—H9	0.9300
N1—C1	1.332 (3)	C10—C10ii	1.439 (4)
N1—C5	1.387 (3)	C10—C11	1.443 (3)
N2—C6	1.368 (3)	C11—C12	1.341 (3)
N2—H2A	0.8600	C11—H11	0.9300
N2—H2B	0.8600	C12—H12	0.9300
N1i—Cd1—N1	180.00 (6)	C2—C1—H1	120.7
N1i—Cd1—O5i	87.37 (7)	C1—C2—C3	119.9 (2)
N1—Cd1—O5i	92.63 (7)	C1—C2—C6	118.8 (2)
N1i—Cd1—O5	92.63 (6)	C3—C2—C6	121.2 (2)
N1—Cd1—O5	87.37 (7)	C4—C3—C2	121.5 (2)
O5i—Cd1—O5	180.0	C4—C3—H3	119.2
N1i—Cd1—O6i	87.44 (7)	C2—C3—H3	119.2
N1—Cd1—O6i	92.56 (7)	C5—C4—C3	115.4 (2)
O5i—Cd1—O6i	86.23 (10)	C5—C4—H4	122.3
O5—Cd1—O6i	93.77 (10)	C3—C4—H4	122.3
N1i—Cd1—O6	92.56 (7)	C4—C5—N1	123.5 (2)
N1—Cd1—O6	87.44 (7)	C4—C5—H5	118.3
O5i—Cd1—O6	93.77 (10)	N1—C5—H5	118.3
O5—Cd1—O6	86.23 (10)	O1—C6—N2	124.3 (2)
O6i—Cd1—O6	180.0	O1—C6—C2	117.0 (2)
O4—S1—O3	114.71 (11)	N2—C6—C2	118.65 (18)
O4—S1—O2	111.55 (16)	C12—C7—C8	123.5 (2)
O3—S1—O2	113.62 (11)	C12—C7—S1	115.34 (19)
O4—S1—C7	106.64 (9)	C8—C7—S1	121.17 (18)
O3—S1—C7	102.88 (13)	C9—C8—C7	119.9 (2)
O2—S1—C7	106.44 (9)	C9—C8—H8	120.1
Cd1—O5—H5A	131.1	C7—C8—H8	120.1
Cd1—O5—H5B	129.3	C8—C9—C10	117.6 (2)
H5A—O5—H5B	97.4	C8—C9—H9	121.2
Cd1—O6—H6A	126.9	C10—C9—H9	121.2
Cd1—O6—H6B	130.0	C9—C10—C10ii	117.4 (3)
H6A—O6—H6B	97.1	C9—C10—C11	121.3 (2)
C1—N1—C5	120.96 (19)	C10ii—C10—C11	121.4 (3)
C1—N1—Cd1	121.05 (16)	C12—C11—C10	121.50 (19)
C5—N1—Cd1	117.99 (15)	C12—C11—H11	119.3
C6—N2—H2A	120.0	C10—C11—H11	119.3
C6—N2—H2B	120.0	C11—C12—C7	116.2 (2)
H2A—N2—H2B	120.0	C11—C12—H12	121.9
N1—C1—C2	118.7 (2)	C7—C12—H12	121.9
N1—C1—H1	120.7

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5A···O3iii	0.81	2.03	2.832 (3)	171
O5—H5B···O4iv	0.86	1.83	2.676 (2)	172
O6—H6A···O3	0.85	1.93	2.777 (3)	178
O6—H6B···O2v	0.83	1.89	2.716 (3)	171
N2—H2A···O1vi	0.86	2.08	2.932 (2)	171
N2—H2B···O2vii	0.86	2.17	3.025 (3)	172

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5A⋯O3i	0.81	2.03	2.832 (3)	171
O5—H5B⋯O4ii	0.86	1.83	2.676 (2)	172
O6—H6A⋯O3	0.85	1.93	2.777 (3)	178
O6—H6B⋯O2iii	0.83	1.89	2.716 (3)	171
N2—H2A⋯O1iv	0.86	2.08	2.932 (2)	171
N2—H2B⋯O2v	0.86	2.17	3.025 (3)	172

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .