Diaqua-bis(9-oxo-4,5-diaza-fluoren-3-olato-κN,O)cadmium(II).

The title compound, [Cd(C(11)H(5)N(2)O(2))(2)(H(2)O)(2)], is a mononuclear complex consisting of a Cd(II) atom, two 3-hydr-oxy-4,5-diaza-fluoren-9-one ligands and two coordinated water mol-ecules. The Cd(II) atom, lying on a twofold axis, displays a distorted octa-hedral coordintion. Adjacent mol-ecules are linked by O-H⋯O hydrogen bonds and π-π inter-actions [centroid-centroid distance = 3.84 (1) Å], leading to a one-dimensional chain. Weak C-H⋯O hydrogen bonds connect the chains into a two-dimensional supra-molecular structure.

Related literature

For related literature, see: Li et al. (2006 ▶); Rillema et al. (2007 ▶); Tershansy et al. (2006 ▶); Zhao et al. (2006 ▶).

Experimental

Crystal data

[Cd(C11H5N2O2)2(H2O)2]

M = 542.77

Monoclinic,

a = 28.190 (5) Å

b = 5.572 (4) Å

c = 13.933 (5) Å

β = 110.622 (5)°

V = 2048.3 (17) Å3

Z = 4

Mo Kα radiation

μ = 1.12 mm−1

T = 293 (2) K

0.26 × 0.21 × 0.17 mm

Data collection

Rigaku R-AXIS RAPID diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.760, T max = 0.833

5972 measured reflections

2406 independent reflections

1965 reflections with I > 2σ(I)

R int = 0.021

Refinement

R[F 2 > 2σ(F 2)] = 0.029

wR(F 2) = 0.082

S = 1.02

2406 reflections

158 parameters

2 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.62 e Å−3

Δρmin = −0.36 e Å−3

Data collection: PROCESS-AUTO (Rigaku, 1998 ▶); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: SHELXTL-Plus (Siemens, 1990 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807067323/hy2109sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807067323/hy2109Isup2.hkl

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

[Cd(C11H5N2O2)2(H2O)2]	F000 = 1080
Mr = 542.77	Dx = 1.760 Mg m−3
Monoclinic, C2/c	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 4465 reflections
a = 28.190 (5) Å	θ = 3.0–28.3º
b = 5.572 (4) Å	µ = 1.12 mm−1
c = 13.933 (5) Å	T = 293 (2) K
β = 110.622 (5)º	Block, colorless
V = 2048.3 (17) Å3	0.26 × 0.21 × 0.17 mm
Z = 4

Rigaku R-AXIS RAPID diffractometer	2406 independent reflections
Radiation source: rotation anode	1965 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.021
T = 293(2) K	θmax = 28.3º
ω scans	θmin = 3.0º
Absorption correction: multi-scan(ABSCOR; Higashi, 1995)	h = −26→37
Tmin = 0.760, Tmax = 0.833	k = −7→7
5972 measured reflections	l = −18→12

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)] = 0.029	H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.082	w = 1/[σ2(Fo2) + (0.0433P)2 + 1.5483P] where P = (Fo2 + 2Fc2)/3
S = 1.02	(Δ/σ)max < 0.001
2406 reflections	Δρmax = 0.62 e Å−3
158 parameters	Δρmin = −0.36 e Å−3
2 restraints	Extinction correction: none
Primary atom site location: structure-invariant direct methods

	x	y	z	Uiso*/Ueq
Cd1	1.0000	0.24267 (5)	0.2500	0.04153 (11)
N1	0.91692 (7)	0.1412 (4)	0.15373 (15)	0.0337 (4)
N2	0.90481 (8)	0.5376 (4)	−0.00770 (16)	0.0400 (5)
O2	0.95401 (7)	−0.0756 (3)	0.29552 (14)	0.0455 (4)
O3	0.75172 (7)	0.0883 (4)	−0.09790 (15)	0.0553 (5)
C1	0.91486 (9)	−0.0461 (4)	0.21600 (18)	0.0358 (5)
C2	0.87029 (11)	−0.1903 (5)	0.1904 (2)	0.0430 (6)
H2	0.8695	−0.3203	0.2317	0.052*
C3	0.82874 (10)	−0.1395 (5)	0.1061 (2)	0.0423 (6)
H3	0.7995	−0.2322	0.0897	0.051*
C4	0.83130 (9)	0.0555 (5)	0.04508 (18)	0.0366 (5)
C5	0.79449 (9)	0.1567 (5)	−0.0489 (2)	0.0404 (6)
C6	0.82108 (9)	0.3654 (5)	−0.07684 (18)	0.0377 (5)
C7	0.80569 (10)	0.5278 (5)	−0.1560 (2)	0.0470 (6)
H7	0.7731	0.5249	−0.2045	0.056*
C8	0.84113 (12)	0.6963 (5)	−0.1601 (2)	0.0501 (7)
H8	0.8325	0.8102	−0.2122	0.060*
C9	0.88918 (12)	0.6950 (5)	−0.0868 (2)	0.0460 (7)
H9	0.9122	0.8091	−0.0920	0.055*
C10	0.87021 (9)	0.3786 (4)	−0.00494 (17)	0.0334 (5)
C11	0.87612 (9)	0.1865 (4)	0.07194 (19)	0.0327 (5)
O1	0.99406 (8)	0.4960 (4)	0.36946 (16)	0.0505 (5)
H1A	1.0223 (8)	0.519 (6)	0.412 (2)	0.065 (10)*
H1B	0.9809 (13)	0.630 (4)	0.353 (3)	0.067 (11)*

	U11	U22	U33	U12	U13	U23
Cd1	0.02980 (15)	0.03837 (17)	0.04841 (18)	0.000	0.00383 (11)	0.000
N1	0.0281 (10)	0.0314 (10)	0.0377 (11)	−0.0028 (8)	0.0066 (8)	0.0013 (9)
N2	0.0387 (11)	0.0401 (12)	0.0400 (11)	−0.0032 (9)	0.0125 (9)	0.0036 (9)
O2	0.0427 (10)	0.0407 (10)	0.0454 (10)	0.0028 (8)	0.0058 (8)	0.0076 (8)
O3	0.0343 (10)	0.0707 (14)	0.0495 (11)	−0.0142 (9)	0.0005 (8)	−0.0081 (10)
C1	0.0369 (12)	0.0317 (12)	0.0382 (13)	0.0023 (10)	0.0124 (10)	0.0002 (10)
C2	0.0489 (16)	0.0348 (13)	0.0490 (15)	−0.0056 (11)	0.0218 (13)	0.0017 (11)
C3	0.0385 (14)	0.0400 (14)	0.0494 (15)	−0.0123 (11)	0.0168 (12)	−0.0068 (12)
C4	0.0296 (11)	0.0403 (13)	0.0385 (13)	−0.0051 (10)	0.0103 (10)	−0.0061 (11)
C5	0.0331 (13)	0.0464 (14)	0.0396 (13)	−0.0031 (11)	0.0100 (11)	−0.0089 (12)
C6	0.0317 (12)	0.0444 (15)	0.0345 (12)	−0.0003 (10)	0.0085 (10)	−0.0048 (11)
C7	0.0415 (14)	0.0581 (17)	0.0355 (13)	0.0076 (12)	0.0062 (11)	0.0035 (12)
C8	0.0597 (18)	0.0509 (16)	0.0383 (14)	0.0123 (14)	0.0154 (13)	0.0101 (12)
C9	0.0500 (16)	0.0423 (15)	0.0499 (16)	0.0011 (12)	0.0227 (13)	0.0083 (12)
C10	0.0318 (11)	0.0350 (13)	0.0312 (11)	−0.0004 (9)	0.0086 (9)	−0.0022 (10)
C11	0.0296 (12)	0.0320 (12)	0.0353 (12)	−0.0025 (9)	0.0097 (10)	−0.0030 (10)
O1	0.0448 (12)	0.0426 (11)	0.0532 (12)	0.0076 (9)	0.0039 (10)	−0.0025 (10)

Cd1—O1	2.233 (2)	C3—C4	1.397 (4)
Cd1—O1i	2.233 (2)	C3—H3	0.9300
Cd1—N1i	2.3217 (19)	C4—C11	1.391 (3)
Cd1—N1	2.3217 (19)	C4—C5	1.468 (4)
Cd1—O2	2.410 (2)	C5—C6	1.507 (4)
Cd1—O2i	2.410 (2)	C6—C7	1.374 (4)
N1—C11	1.327 (3)	C6—C10	1.396 (3)
N1—C1	1.371 (3)	C7—C8	1.386 (4)
N2—C10	1.328 (3)	C7—H7	0.9300
N2—C9	1.355 (3)	C8—C9	1.380 (4)
O2—C1	1.269 (3)	C8—H8	0.9300
O3—C5	1.219 (3)	C9—H9	0.9300
C1—C2	1.427 (4)	C10—C11	1.482 (4)
C2—C3	1.365 (4)	O1—H1A	0.817 (18)
C2—H2	0.9300	O1—H1B	0.832 (19)
O1—Cd1—O1i	101.59 (13)	C4—C3—H3	120.9
O1—Cd1—N1i	92.77 (7)	C11—C4—C3	118.8 (2)
O1i—Cd1—N1i	105.03 (8)	C11—C4—C5	109.1 (2)
O1—Cd1—N1	105.03 (8)	C3—C4—C5	132.1 (2)
O1i—Cd1—N1	92.77 (7)	O3—C5—C4	128.9 (3)
N1i—Cd1—N1	151.82 (11)	O3—C5—C6	125.5 (3)
O1—Cd1—O2	94.62 (9)	C4—C5—C6	105.5 (2)
O1i—Cd1—O2	148.19 (7)	C7—C6—C10	119.6 (2)
N1i—Cd1—O2	101.27 (7)	C7—C6—C5	132.1 (2)
N1—Cd1—O2	56.38 (7)	C10—C6—C5	108.3 (2)
O1—Cd1—O2i	148.19 (7)	C6—C7—C8	116.8 (2)
O1i—Cd1—O2i	94.62 (9)	C6—C7—H7	121.6
N1i—Cd1—O2i	56.38 (7)	C8—C7—H7	121.6
N1—Cd1—O2i	101.27 (7)	C9—C8—C7	120.0 (3)
O2—Cd1—O2i	85.23 (11)	C9—C8—H8	120.0
C11—N1—C1	118.1 (2)	C7—C8—H8	120.0
C11—N1—Cd1	147.41 (17)	N2—C9—C8	124.0 (3)
C1—N1—Cd1	94.51 (14)	N2—C9—H9	118.0
C10—N2—C9	115.1 (2)	C8—C9—H9	118.0
C1—O2—Cd1	93.31 (15)	N2—C10—C6	124.6 (2)
O2—C1—N1	115.7 (2)	N2—C10—C11	127.3 (2)
O2—C1—C2	124.3 (2)	C6—C10—C11	108.1 (2)
N1—C1—C2	120.0 (2)	N1—C11—C4	124.2 (2)
C3—C2—C1	120.8 (3)	N1—C11—C10	126.9 (2)
C3—C2—H2	119.6	C4—C11—C10	108.9 (2)
C1—C2—H2	119.6	Cd1—O1—H1A	109 (2)
C2—C3—C4	118.2 (2)	Cd1—O1—H1B	120 (2)
C2—C3—H3	120.9	H1A—O1—H1B	107 (3)
O1—Cd1—N1—C11	93.5 (3)	C3—C4—C5—C6	−179.4 (3)
O1i—Cd1—N1—C11	−9.3 (3)	O3—C5—C6—C7	2.3 (5)
N1i—Cd1—N1—C11	−139.1 (3)	C4—C5—C6—C7	−179.5 (3)
O2—Cd1—N1—C11	179.0 (3)	O3—C5—C6—C10	−176.9 (3)
O2i—Cd1—N1—C11	−104.6 (3)	C4—C5—C6—C10	1.4 (3)
O1—Cd1—N1—C1	−87.51 (16)	C10—C6—C7—C8	0.9 (4)
O1i—Cd1—N1—C1	169.70 (14)	C5—C6—C7—C8	−178.2 (3)
N1i—Cd1—N1—C1	39.89 (13)	C6—C7—C8—C9	0.1 (4)
O2—Cd1—N1—C1	−2.01 (13)	C10—N2—C9—C8	0.3 (4)
O2i—Cd1—N1—C1	74.44 (15)	C7—C8—C9—N2	−0.7 (5)
O1—Cd1—O2—C1	107.16 (15)	C9—N2—C10—C6	0.7 (4)
O1i—Cd1—O2—C1	−13.7 (2)	C9—N2—C10—C11	−179.8 (2)
N1i—Cd1—O2—C1	−159.08 (14)	C7—C6—C10—N2	−1.3 (4)
N1—Cd1—O2—C1	2.17 (14)	C5—C6—C10—N2	178.0 (2)
O2i—Cd1—O2—C1	−104.75 (16)	C7—C6—C10—C11	179.0 (2)
Cd1—O2—C1—N1	−3.4 (2)	C5—C6—C10—C11	−1.7 (3)
Cd1—O2—C1—C2	177.7 (2)	C1—N1—C11—C4	−0.2 (4)
C11—N1—C1—O2	−177.1 (2)	Cd1—N1—C11—C4	178.7 (2)
Cd1—N1—C1—O2	3.5 (2)	C1—N1—C11—C10	−180.0 (2)
C11—N1—C1—C2	1.9 (3)	Cd1—N1—C11—C10	−1.1 (5)
Cd1—N1—C1—C2	−177.5 (2)	C3—C4—C11—N1	−1.3 (4)
O2—C1—C2—C3	176.7 (2)	C5—C4—C11—N1	179.7 (2)
N1—C1—C2—C3	−2.2 (4)	C3—C4—C11—C10	178.6 (2)
C1—C2—C3—C4	0.7 (4)	C5—C4—C11—C10	−0.5 (3)
C2—C3—C4—C11	0.9 (4)	N2—C10—C11—N1	1.6 (4)
C2—C3—C4—C5	179.7 (3)	C6—C10—C11—N1	−178.8 (2)
C11—C4—C5—O3	177.7 (3)	N2—C10—C11—C4	−178.3 (2)
C3—C4—C5—O3	−1.2 (5)	C6—C10—C11—C4	1.4 (3)
C11—C4—C5—C6	−0.5 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···N2i	0.82 (2)	2.02 (2)	2.832 (3)	172 (3)
O1—H1B···O2ii	0.83 (2)	1.86 (2)	2.686 (3)	170 (4)
C3—H3···O3iii	0.93	2.48	3.351 (5)	156

Cd1—O1	2.233 (2)
Cd1—N1	2.3217 (19)
Cd1—O2	2.410 (2)

O1—Cd1—O1i	101.59 (13)
O1—Cd1—N1i	92.77 (7)
O1—Cd1—N1	105.03 (8)
N1i—Cd1—N1	151.82 (11)
O1—Cd1—O2	94.62 (9)
O1i—Cd1—O2	148.19 (7)
N1i—Cd1—O2	101.27 (7)
N1—Cd1—O2	56.38 (7)
O2—Cd1—O2i	85.23 (11)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯N2i	0.82 (2)	2.02 (2)	2.832 (3)	172 (3)
O1—H1B⋯O2ii	0.83 (2)	1.86 (2)	2.686 (3)	170 (4)
C3—H3⋯O3iii	0.93	2.48	3.351 (5)	156

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