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In the centrosymmetric binuclear title complex, [Cd2(C6H8O4)(NO3)2(C14H12N2)2(H2O)2], each Cd atom is seven-coordinated in a CdO5N2 environment with a distorted petagonal-bipyramidal geometry. The water mol­ecules act as both donors and acceptors in O—H...O hydrogen bonds, inter­connecting the mol­ecules into double chains along the b axis. The packing is further stabilized by π–π inter­actions between the phenanthroline ring systems.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805029533/cv6578sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805029533/cv6578Isup2.hkl
Contains datablock I

CCDC reference: 287543

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.027
  • wR factor = 0.068
  • Data-to-parameter ratio = 13.9

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cd1 - O2 .. 15.05 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cd1 - O3 .. 19.90 su
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cd1 - O4 .. 7.79 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O3 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O4 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N3 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C14 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 52 O1W -CD1 -C15 -C16 142.60 1.60 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 53 O4 -CD1 -C15 -C16 52.40 1.50 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 54 N1 -CD1 -C15 -C16 -107.50 1.60 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 55 N2 -CD1 -C15 -C16 -31.90 1.60 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 56 O2 -CD1 -C15 -C16 64.20 1.60 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 57 O5 -CD1 -C15 -C16 -132.10 1.70 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 58 O3 -CD1 -C15 -C16 53.60 1.70 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 92 CD1 -C15 -C16 -C17 115.70 1.50 1.555 1.555 1.555 1.555 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 18 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 11 ALERT type 4 Improvement, methodology, query or suggestion

Comment top

Recently, we reported the structure of di-µ-adipato-κ6O,O':O'';O:O',O''-bis[aqua(1,10-phenanthroline-κ2N,N)zinc(II)] (Ding et al., 2005). In our ongoing studies, we synthesized the title compound, (I). An X-ray crystallographic analysis was undertaken to determine the stereochemistry of (I).

The binuclear cadmium complex molecule in (I) possesses a crystallographically imposed centre of symmetry (Fig. 1). Each CdII atom is seven-coordinated by two N atoms and five O atoms (Table 1) in a distorted petagonal–bipyramidal geometry. One axial position is occupied by atom O1W of the water molecule, with a Cd—O distance of 2.283 (2) Å. The other axial position is occupied by atom N2 of the 2,9-dimethylphenanthroline ligand.

In the crystal structure, the water molecules act as both donors and acceptors to form O—H···O hydrogen bonds (Table 2). These hydrogen bonds link the molecules into double chains along the c axis (Fig. 2). The short Cg1···Cg1i distance of 3.508 (2) Å [Cg1 is the centroid of the C4–C7/C11/C12 ring; symmetry code: (i) 1 − x, y, 1/2 − z] indicates an existence of ππ stacking interactions between the tricycles, which stabilize the packing.

Experimental top

To a solution of 2,9-dimethyl-1,10-phenanthroline (0.21 g, 1 mmol) and adipic acid (0.73 g, 0.5 mmol) in ethanol (10 ml) was added a solution of cadmium nitrate (0.31 g, 1 mmol) in distilled water (10 ml). The mixture was stirred and refluxed for 2 h. The hot solution was then filtered into another flask containing ethanol (10 ml). Orange crystals appeared over a period of one week by slow evaporation at room temperature.

Refinement top

C-bound H atoms were positioned geometrically and allowed to ride on their parent atoms, with C—H = 0.93–0.97 Å and Uiso(H) = 1.2–1.5Ueq(parent atom). The H atoms of the water molecules were located in a difference Fourier map and refined isotropically.

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 2003).

Figures top
[Figure 1] Fig. 1. View of (I), showing the atom-numbering scheme and 50% probability displacement ellipsoids. H atoms have been omitted for clarity. Unlabelled atoms are related to labelled atoms by the symmetry code (−x, −y, −z).
[Figure 2] Fig. 2. Packing diagram of (I), viewed approximately down the b axis. Intermolecular hydrogen bonds are denoted by dashed lines.
µ-Adipato-κ4O,O':O'',O'''-bis[aqua(2,9-dimethyl-1,10-phenanthroline- κ2N,N)nitratocadmium(II)] dihydrate top
Crystal data top
[Cd2(C6H8O4)(NO3)2(C14H12N2)2(H2O)2]F(000) = 1976
Mr = 981.54Dx = 1.724 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 24.438 (2) ÅCell parameters from 5950 reflections
b = 11.2315 (10) Åθ = 2.4–26.1°
c = 13.8799 (12) ŵ = 1.20 mm1
β = 96.969 (1)°T = 293 K
V = 3781.6 (6) Å3Column, orange
Z = 40.30 × 0.16 × 0.07 mm
Data collection top
Siemens SMART 1000 CCD area-detector
diffractometer
3730 independent reflections
Radiation source: fine-focus sealed tube3367 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.016
Detector resolution: 8.33 pixels mm-1θmax = 26.1°, θmin = 1.7°
ω scansh = 2630
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 813
Tmin = 0.715, Tmax = 0.921l = 1716
10344 measured reflections
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)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.068H atoms treated by a mixture of independent and constrained refinement
S = 1.05 w = 1/[σ2(Fo2) + (0.0341P)2 + 4.9157P]
where P = (Fo2 + 2Fc2)/3
3730 reflections(Δ/σ)max = 0.001
269 parametersΔρmax = 0.48 e Å3
0 restraintsΔρmin = 0.29 e Å3
Crystal data top
[Cd2(C6H8O4)(NO3)2(C14H12N2)2(H2O)2]V = 3781.6 (6) Å3
Mr = 981.54Z = 4
Monoclinic, C2/cMo Kα radiation
a = 24.438 (2) ŵ = 1.20 mm1
b = 11.2315 (10) ÅT = 293 K
c = 13.8799 (12) Å0.30 × 0.16 × 0.07 mm
β = 96.969 (1)°
Data collection top
Siemens SMART 1000 CCD area-detector
diffractometer
3730 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
3367 reflections with I > 2σ(I)
Tmin = 0.715, Tmax = 0.921Rint = 0.016
10344 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0270 restraints
wR(F2) = 0.068H atoms treated by a mixture of independent and constrained refinement
S = 1.05Δρmax = 0.48 e Å3
3730 reflectionsΔρmin = 0.29 e Å3
269 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
Cd10.350986 (7)0.222427 (17)0.404857 (12)0.03725 (8)
O50.31775 (7)0.16749 (18)0.23561 (12)0.0457 (4)
N10.43205 (8)0.1215 (2)0.38421 (14)0.0394 (5)
O1W0.28862 (10)0.0892 (2)0.45124 (18)0.0545 (5)
O40.28045 (9)0.3150 (2)0.30520 (14)0.0588 (5)
C40.52960 (11)0.1474 (4)0.37510 (18)0.0549 (8)
O30.39925 (10)0.2337 (2)0.58077 (18)0.0686 (6)
N30.36264 (12)0.2990 (2)0.60722 (18)0.0570 (7)
C150.28502 (11)0.2523 (2)0.23148 (19)0.0414 (6)
N20.41812 (9)0.3679 (2)0.38743 (14)0.0434 (5)
O20.32299 (9)0.3256 (2)0.54418 (15)0.0622 (5)
C70.51523 (13)0.3962 (3)0.3747 (2)0.0586 (9)
C120.47638 (10)0.1941 (3)0.38105 (17)0.0432 (6)
C160.25123 (13)0.2861 (3)0.1378 (2)0.0590 (8)
H16A0.25260.37200.13140.071*
H16B0.21320.26460.14250.071*
C50.57482 (13)0.2254 (4)0.3691 (2)0.0708 (11)
H5A0.60970.19370.36570.085*
C170.26777 (13)0.2313 (3)0.0458 (2)0.0532 (7)
H17A0.30570.25290.04030.080*
H17B0.26620.14530.05140.080*
C10.43836 (12)0.0037 (3)0.37968 (18)0.0475 (7)
C110.46922 (11)0.3224 (3)0.38166 (17)0.0445 (6)
C130.38890 (13)0.0733 (3)0.3787 (2)0.0590 (8)
H13A0.35690.02450.38150.089*
H13B0.39340.12560.43380.089*
H13C0.38440.11970.32020.089*
C90.45471 (17)0.5631 (3)0.3769 (2)0.0700 (10)
H9A0.44880.64490.37450.084*
C100.41070 (13)0.4858 (3)0.3856 (2)0.0534 (7)
C20.49046 (13)0.0473 (3)0.3751 (2)0.0591 (8)
H2A0.49410.12970.37330.071*
C80.50601 (16)0.5191 (4)0.3720 (2)0.0726 (11)
H8A0.53520.57100.36680.087*
O10.36506 (14)0.3354 (4)0.68990 (19)0.1108 (11)
C30.53512 (13)0.0224 (4)0.3732 (2)0.0625 (9)
H3A0.56960.01170.37070.075*
O2W0.30667 (11)0.0534 (3)0.64346 (18)0.0644 (6)
C140.35495 (14)0.5343 (3)0.3939 (2)0.0643 (9)
H14A0.32980.46980.39960.096*
H14B0.34260.58020.33700.096*
H14C0.35640.58420.45030.096*
C60.56816 (13)0.3436 (5)0.3684 (2)0.0716 (11)
H6A0.59840.39260.36380.086*
H2W10.2546 (18)0.110 (4)0.435 (3)0.098 (15)*
H2W20.3072 (15)0.010 (4)0.670 (3)0.077 (13)*
H1W10.2946 (15)0.076 (4)0.509 (3)0.078 (13)*
H1W20.279 (2)0.099 (5)0.661 (4)0.14 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.03456 (12)0.04430 (13)0.03231 (11)0.00217 (8)0.00174 (7)0.00127 (7)
O50.0458 (10)0.0537 (12)0.0356 (9)0.0082 (9)0.0034 (7)0.0006 (8)
N10.0361 (11)0.0513 (13)0.0294 (10)0.0051 (10)0.0013 (8)0.0002 (9)
O1W0.0546 (13)0.0576 (13)0.0533 (13)0.0033 (11)0.0149 (10)0.0048 (11)
O40.0714 (14)0.0598 (13)0.0416 (11)0.0192 (11)0.0073 (9)0.0082 (10)
C40.0363 (14)0.099 (3)0.0283 (12)0.0034 (15)0.0004 (10)0.0023 (14)
O30.0562 (14)0.0897 (18)0.0601 (14)0.0053 (12)0.0082 (11)0.0096 (12)
N30.0638 (17)0.0648 (17)0.0424 (14)0.0182 (14)0.0070 (12)0.0122 (12)
C150.0430 (14)0.0483 (16)0.0308 (13)0.0018 (12)0.0043 (11)0.0009 (11)
N20.0490 (13)0.0488 (13)0.0316 (10)0.0062 (10)0.0016 (9)0.0029 (9)
O20.0574 (13)0.0775 (15)0.0522 (12)0.0063 (12)0.0084 (10)0.0018 (11)
C70.0547 (18)0.088 (3)0.0321 (14)0.0268 (17)0.0001 (12)0.0023 (14)
C120.0367 (13)0.0690 (19)0.0228 (11)0.0001 (12)0.0002 (9)0.0008 (11)
C160.0567 (18)0.071 (2)0.0446 (16)0.0185 (16)0.0112 (14)0.0052 (14)
C50.0344 (16)0.136 (4)0.0418 (17)0.0040 (19)0.0030 (12)0.004 (2)
C170.0523 (17)0.067 (2)0.0370 (15)0.0106 (14)0.0063 (13)0.0024 (13)
C10.0507 (15)0.0567 (18)0.0330 (13)0.0138 (14)0.0034 (11)0.0022 (12)
C110.0416 (14)0.0675 (18)0.0235 (11)0.0105 (13)0.0005 (10)0.0019 (12)
C130.0609 (18)0.0466 (17)0.0671 (19)0.0056 (15)0.0024 (15)0.0007 (15)
C90.095 (3)0.057 (2)0.0560 (19)0.025 (2)0.0030 (18)0.0066 (16)
C100.072 (2)0.0504 (17)0.0372 (14)0.0129 (15)0.0016 (13)0.0045 (12)
C20.0579 (19)0.071 (2)0.0459 (16)0.0255 (17)0.0014 (13)0.0061 (15)
C80.083 (3)0.086 (3)0.0472 (17)0.046 (2)0.0008 (16)0.0069 (17)
O10.131 (3)0.150 (3)0.0516 (15)0.022 (2)0.0094 (15)0.0447 (18)
C30.0464 (17)0.100 (3)0.0399 (15)0.0270 (18)0.0022 (12)0.0072 (16)
O2W0.0801 (17)0.0564 (15)0.0588 (14)0.0042 (13)0.0162 (12)0.0120 (12)
C140.087 (2)0.0419 (17)0.064 (2)0.0046 (16)0.0087 (18)0.0033 (14)
C60.0449 (18)0.127 (4)0.0418 (16)0.031 (2)0.0023 (13)0.003 (2)
Geometric parameters (Å, º) top
Cd1—O1W2.283 (2)C16—C171.516 (4)
Cd1—O42.321 (2)C16—H16A0.9700
Cd1—N12.330 (2)C16—H16B0.9700
Cd1—N22.348 (2)C5—C61.338 (6)
Cd1—O22.423 (2)C5—H5A0.9300
Cd1—O52.4690 (17)C17—C17i1.511 (5)
Cd1—O32.583 (3)C17—H17A0.9700
Cd1—C152.750 (3)C17—H17B0.9700
O5—C151.240 (3)C1—C21.405 (4)
N1—C11.335 (4)C1—C131.485 (4)
N1—C121.361 (3)C13—H13A0.9600
O1W—H2W10.87 (4)C13—H13B0.9600
O1W—H1W10.81 (4)C13—H13C0.9600
O4—C151.258 (3)C9—C81.357 (5)
C4—C31.411 (5)C9—C101.399 (4)
C4—C121.414 (4)C9—H9A0.9300
C4—C51.420 (5)C10—C141.484 (4)
O3—N31.247 (4)C2—C31.346 (5)
N3—O11.213 (3)C2—H2A0.9300
N3—O21.260 (3)C8—H8A0.9300
C15—C161.502 (4)C3—H3A0.9300
N2—C101.337 (4)O2W—H2W20.80 (4)
N2—C111.361 (4)O2W—H1W20.90 (6)
C7—C81.398 (5)C14—H14A0.9600
C7—C111.410 (4)C14—H14B0.9600
C7—C61.434 (5)C14—H14C0.9600
C12—C111.452 (4)C6—H6A0.9300
O1W—Cd1—O489.34 (9)N1—C12—C4121.4 (3)
O1W—Cd1—N1108.81 (8)N1—C12—C11119.8 (2)
O4—Cd1—N1136.52 (7)C4—C12—C11118.7 (3)
O1W—Cd1—N2169.53 (8)C15—C16—C17116.8 (2)
O4—Cd1—N296.01 (8)C15—C16—H16A108.1
N1—Cd1—N273.19 (8)C17—C16—H16A108.1
O1W—Cd1—O279.95 (8)C15—C16—H16B108.1
O4—Cd1—O290.02 (7)C17—C16—H16B108.1
N1—Cd1—O2131.10 (7)H16A—C16—H16B107.3
N2—Cd1—O291.03 (8)C6—C5—C4121.2 (3)
O1W—Cd1—O587.17 (8)C6—C5—H5A119.4
O4—Cd1—O553.84 (7)C4—C5—H5A119.4
N1—Cd1—O587.02 (6)C17i—C17—C16114.3 (3)
N2—Cd1—O5103.25 (7)C17i—C17—H17A108.7
O2—Cd1—O5141.87 (7)C16—C17—H17A108.7
O1W—Cd1—O390.54 (9)C17i—C17—H17B108.7
O4—Cd1—O3139.69 (8)C16—C17—H17B108.7
N1—Cd1—O380.93 (7)H17A—C17—H17B107.6
N2—Cd1—O379.56 (7)N1—C1—C2121.1 (3)
O2—Cd1—O350.43 (8)N1—C1—C13118.6 (2)
O5—Cd1—O3166.29 (7)C2—C1—C13120.2 (3)
O1W—Cd1—C1589.21 (9)N2—C11—C7121.9 (3)
O4—Cd1—C1527.08 (8)N2—C11—C12119.0 (2)
N1—Cd1—C15111.63 (8)C7—C11—C12119.1 (3)
N2—Cd1—C1599.66 (8)C1—C13—H13A109.5
O2—Cd1—C15116.61 (8)C1—C13—H13B109.5
O5—Cd1—C1526.81 (7)H13A—C13—H13B109.5
O3—Cd1—C15166.77 (8)C1—C13—H13C109.5
C15—O5—Cd189.31 (15)H13A—C13—H13C109.5
C1—N1—C12119.7 (2)H13B—C13—H13C109.5
C1—N1—Cd1126.37 (18)C8—C9—C10120.2 (4)
C12—N1—Cd1113.87 (18)C8—C9—H9A119.9
Cd1—O1W—H2W1114 (3)C10—C9—H9A119.9
Cd1—O1W—H1W1111 (3)N2—C10—C9120.8 (3)
H2W1—O1W—H1W1111 (4)N2—C10—C14119.0 (3)
C15—O4—Cd195.82 (17)C9—C10—C14120.1 (3)
C3—C4—C12117.4 (3)C3—C2—C1120.3 (3)
C3—C4—C5122.4 (3)C3—C2—H2A119.8
C12—C4—C5120.2 (3)C1—C2—H2A119.8
N3—O3—Cd192.60 (17)C9—C8—C7120.3 (3)
O1—N3—O3121.5 (3)C9—C8—H8A119.8
O1—N3—O2121.5 (3)C7—C8—H8A119.8
O3—N3—O2117.0 (2)C2—C3—C4119.9 (3)
O5—C15—O4120.8 (2)C2—C3—H3A120.0
O5—C15—C16121.2 (2)C4—C3—H3A120.0
O4—C15—C16117.9 (3)H2W2—O2W—H1W2111 (4)
O5—C15—Cd163.88 (13)C10—C14—H14A109.5
O4—C15—Cd157.11 (13)C10—C14—H14B109.5
C16—C15—Cd1172.2 (2)H14A—C14—H14B109.5
C10—N2—C11119.6 (3)C10—C14—H14C109.5
C10—N2—Cd1126.6 (2)H14A—C14—H14C109.5
C11—N2—Cd1113.75 (19)H14B—C14—H14C109.5
N3—O2—Cd199.97 (17)C5—C6—C7121.2 (3)
C8—C7—C11117.1 (3)C5—C6—H6A119.4
C8—C7—C6123.3 (3)C7—C6—H6A119.4
C11—C7—C6119.7 (4)
O1W—Cd1—O5—C1593.84 (17)C15—Cd1—N2—C1067.6 (2)
O4—Cd1—O5—C152.58 (17)O1W—Cd1—N2—C1198.1 (5)
N1—Cd1—O5—C15157.15 (17)O4—Cd1—N2—C11141.40 (16)
N2—Cd1—O5—C1585.20 (17)N1—Cd1—N2—C114.48 (16)
O2—Cd1—O5—C1524.1 (2)O2—Cd1—N2—C11128.47 (17)
O3—Cd1—O5—C15174.5 (3)O5—Cd1—N2—C1187.18 (16)
O1W—Cd1—N1—C113.0 (2)O3—Cd1—N2—C1179.10 (17)
O4—Cd1—N1—C197.0 (2)C15—Cd1—N2—C11114.31 (17)
N2—Cd1—N1—C1177.8 (2)O1—N3—O2—Cd1179.1 (3)
O2—Cd1—N1—C1106.0 (2)O3—N3—O2—Cd10.9 (3)
O5—Cd1—N1—C173.0 (2)O1W—Cd1—O2—N399.65 (19)
O3—Cd1—N1—C1100.5 (2)O4—Cd1—O2—N3171.02 (19)
C15—Cd1—N1—C183.9 (2)N1—Cd1—O2—N36.6 (2)
O1W—Cd1—N1—C12164.07 (16)N2—Cd1—O2—N375.00 (18)
O4—Cd1—N1—C1285.95 (19)O5—Cd1—O2—N3171.78 (15)
N2—Cd1—N1—C125.14 (16)O3—Cd1—O2—N30.52 (17)
O2—Cd1—N1—C1271.06 (19)C15—Cd1—O2—N3176.34 (17)
O5—Cd1—N1—C12109.94 (16)C1—N1—C12—C41.4 (3)
O3—Cd1—N1—C1276.61 (16)Cd1—N1—C12—C4175.92 (18)
C15—Cd1—N1—C1299.08 (17)C1—N1—C12—C11177.3 (2)
O1W—Cd1—O4—C1589.54 (19)Cd1—N1—C12—C115.4 (3)
N1—Cd1—O4—C1527.6 (2)C3—C4—C12—N10.4 (4)
N2—Cd1—O4—C1599.47 (19)C5—C4—C12—N1178.2 (2)
O2—Cd1—O4—C15169.49 (19)C3—C4—C12—C11179.1 (2)
O5—Cd1—O4—C152.56 (16)C5—C4—C12—C110.5 (4)
O3—Cd1—O4—C15179.59 (17)O5—C15—C16—C1713.2 (5)
O1W—Cd1—O3—N376.98 (18)O4—C15—C16—C17164.6 (3)
O4—Cd1—O3—N312.6 (2)Cd1—C15—C16—C17115.7 (15)
N1—Cd1—O3—N3174.05 (19)C3—C4—C5—C6178.2 (3)
N2—Cd1—O3—N399.62 (19)C12—C4—C5—C60.4 (4)
O2—Cd1—O3—N30.52 (17)C15—C16—C17—C17i180.0 (4)
O5—Cd1—O3—N3157.2 (3)C12—N1—C1—C22.2 (4)
C15—Cd1—O3—N311.8 (5)Cd1—N1—C1—C2174.68 (19)
Cd1—O3—N3—O1179.2 (3)C12—N1—C1—C13177.2 (2)
Cd1—O3—N3—O20.9 (3)Cd1—N1—C1—C135.9 (3)
Cd1—O5—C15—O44.5 (3)C10—N2—C11—C70.6 (4)
Cd1—O5—C15—C16173.2 (3)Cd1—N2—C11—C7177.59 (18)
Cd1—O4—C15—O54.8 (3)C10—N2—C11—C12178.3 (2)
Cd1—O4—C15—C16173.0 (2)Cd1—N2—C11—C123.5 (3)
O1W—Cd1—C15—O585.30 (17)C8—C7—C11—N21.2 (4)
O4—Cd1—C15—O5175.4 (3)C6—C7—C11—N2179.8 (2)
N1—Cd1—C15—O524.66 (18)C8—C7—C11—C12177.8 (2)
N2—Cd1—C15—O5100.29 (17)C6—C7—C11—C120.8 (4)
O2—Cd1—C15—O5163.65 (15)N1—C12—C11—N21.3 (3)
O3—Cd1—C15—O5174.3 (3)C4—C12—C11—N2180.0 (2)
O1W—Cd1—C15—O490.11 (19)N1—C12—C11—C7177.6 (2)
N1—Cd1—C15—O4159.92 (18)C4—C12—C11—C71.1 (3)
N2—Cd1—C15—O484.29 (19)C11—N2—C10—C90.6 (4)
O2—Cd1—C15—O411.8 (2)Cd1—N2—C10—C9178.6 (2)
O5—Cd1—C15—O4175.4 (3)C11—N2—C10—C14178.8 (2)
O3—Cd1—C15—O41.2 (5)Cd1—N2—C10—C140.9 (4)
O1W—Cd1—C15—C16142.6 (16)C8—C9—C10—N21.2 (5)
O4—Cd1—C15—C1652.4 (15)C8—C9—C10—C14178.2 (3)
N1—Cd1—C15—C16107.5 (16)N1—C1—C2—C31.3 (4)
N2—Cd1—C15—C1631.9 (16)C13—C1—C2—C3178.1 (3)
O2—Cd1—C15—C1664.2 (16)C10—C9—C8—C70.6 (5)
O5—Cd1—C15—C16132.1 (17)C11—C7—C8—C90.6 (4)
O3—Cd1—C15—C1653.6 (17)C6—C7—C8—C9179.1 (3)
O1W—Cd1—N2—C1079.9 (5)C1—C2—C3—C40.5 (4)
O4—Cd1—N2—C1040.5 (2)C12—C4—C3—C21.3 (4)
N1—Cd1—N2—C10177.4 (2)C5—C4—C3—C2177.3 (3)
O2—Cd1—N2—C1049.6 (2)C4—C5—C6—C70.7 (5)
O5—Cd1—N2—C1094.7 (2)C8—C7—C6—C5178.5 (3)
O3—Cd1—N2—C1099.0 (2)C11—C7—C6—C50.0 (4)
Symmetry code: (i) x+1/2, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O2W0.81 (4)1.87 (4)2.681 (4)177 (4)
O2W—H1W2···O4ii0.90 (5)1.85 (5)2.756 (4)177 (5)
O2W—H2W2···O5iii0.80 (4)1.99 (4)2.789 (4)173 (4)
C14—H14B···O1iv0.962.373.223 (4)147
Symmetry codes: (ii) x+1/2, y+1/2, z+1; (iii) x, y, z+1/2; (iv) x, y+1, z1/2.

Experimental details

Crystal data
Chemical formula[Cd2(C6H8O4)(NO3)2(C14H12N2)2(H2O)2]
Mr981.54
Crystal system, space groupMonoclinic, C2/c
Temperature (K)293
a, b, c (Å)24.438 (2), 11.2315 (10), 13.8799 (12)
β (°) 96.969 (1)
V3)3781.6 (6)
Z4
Radiation typeMo Kα
µ (mm1)1.20
Crystal size (mm)0.30 × 0.16 × 0.07
Data collection
DiffractometerSiemens SMART 1000 CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.715, 0.921
No. of measured, independent and
observed [I > 2σ(I)] reflections
10344, 3730, 3367
Rint0.016
(sin θ/λ)max1)0.618
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.027, 0.068, 1.05
No. of reflections3730
No. of parameters269
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.48, 0.29

Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SAINT, SHELXTL (Sheldrick, 1997), SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 2003).

Selected bond lengths (Å) top
Cd1—O1W2.283 (2)Cd1—O22.423 (2)
Cd1—O42.321 (2)Cd1—O52.4690 (17)
Cd1—N12.330 (2)Cd1—O32.583 (3)
Cd1—N22.348 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O2W0.81 (4)1.87 (4)2.681 (4)177 (4)
O2W—H1W2···O4i0.90 (5)1.85 (5)2.756 (4)177 (5)
O2W—H2W2···O5ii0.80 (4)1.99 (4)2.789 (4)173 (4)
C14—H14B···O1iii0.962.373.223 (4)147
Symmetry codes: (i) x+1/2, y+1/2, z+1; (ii) x, y, z+1/2; (iii) x, y+1, z1/2.
 

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