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In the title compound, {[Cd(C7H3NO4)(C14H8N4)]·H2O}n, the CdII atom is seven-coordinated by three N atoms from one pyrazino[2,3-f][1,10]phenanthroline mol­ecule and one pyridine-2,5-dicarboxyl­ate (2,5-pdc) ligand, and four O atoms from three different 2,5-pdc anions in a distorted monocapped octa­hedral coordination geometry. The CdII atoms are bridged by the 2,5-pdc ligands, forming a layer.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806045600/ng2138sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806045600/ng2138Isup2.hkl
Contains datablock I

CCDC reference: 630181

Key indicators

  • Single-crystal X-ray study
  • T = 292 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.023
  • wR factor = 0.068
  • Data-to-parameter ratio = 15.1

checkCIF/PLATON results

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Alert level C PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

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 (Sheldrick, 1990); software used to prepare material for publication: SHELXL97.

Poly[[[(pyrazino[2,3-f][1,10]phenanthroline-κ2N,N')cadmium(II)]- µ3-pyridine-2,5-dicarboxylato-κ3O,O':N,O:O'':O''] monohydrate] top
Crystal data top
[Cd(C7H3NO4)(C14H8N4)]·H2OF(000) = 1048
Mr = 527.76Dx = 1.792 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 15845 reflections
a = 10.754 (2) Åθ = 3.0–27.5°
b = 10.631 (2) ŵ = 1.16 mm1
c = 17.127 (3) ÅT = 292 K
β = 92.64 (3)°Block, colorless
V = 1956.0 (6) Å30.30 × 0.27 × 0.23 mm
Z = 4
Data collection top
Rigaku R-AXIS RAPID
diffractometer
4451 independent reflections
Radiation source: rotorating anode3937 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
Detector resolution: 10.0 pixels mm-1θmax = 27.5°, θmin = 3.1°
ω scansh = 1313
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1313
Tmin = 0.670, Tmax = 0.763l = 2222
18518 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)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.068H atoms treated by a mixture of independent and constrained refinement
S = 1.12 w = 1/[σ2(Fo2) + (0.0334P)2 + 1.031P]
where P = (Fo2 + 2Fc2)/3
4451 reflections(Δ/σ)max = 0.001
295 parametersΔρmax = 0.50 e Å3
4 restraintsΔρmin = 0.46 e Å3
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
C10.2914 (2)0.5276 (2)0.42112 (14)0.0345 (5)
C20.3012 (2)0.6218 (2)0.35508 (13)0.0309 (5)
C30.2017 (2)0.6489 (3)0.30362 (15)0.0414 (6)
H30.12560.60870.30840.050*
C40.2168 (2)0.7365 (3)0.24508 (14)0.0411 (6)
H40.15120.75550.20980.049*
C50.3308 (2)0.7957 (2)0.23974 (13)0.0320 (5)
C60.4253 (2)0.7629 (2)0.29347 (13)0.0323 (5)
H60.50220.80220.29020.039*
C70.3541 (3)0.8960 (3)0.18007 (15)0.0423 (6)
C80.7856 (2)0.7010 (3)0.29796 (14)0.0405 (6)
H80.76430.62800.27060.049*
C90.8759 (3)0.7793 (3)0.26906 (15)0.0459 (6)
H90.91380.75860.22310.055*
C100.9086 (3)0.8865 (3)0.30826 (16)0.0444 (6)
H100.96970.93920.28960.053*
C110.8494 (2)0.9168 (2)0.37710 (15)0.0345 (5)
C120.7584 (2)0.8331 (2)0.40217 (13)0.0302 (5)
C130.6922 (2)0.8613 (2)0.47268 (13)0.0315 (5)
C140.5440 (3)0.8029 (3)0.55828 (17)0.0533 (7)
H140.48310.74670.57300.064*
C150.5671 (4)0.9091 (3)0.6039 (2)0.0640 (10)
H150.52320.92290.64870.077*
C160.6543 (3)0.9922 (3)0.58231 (18)0.0566 (8)
H160.67071.06380.61230.068*
C170.7198 (2)0.9707 (2)0.51491 (15)0.0396 (5)
C180.8152 (3)1.0561 (2)0.48922 (16)0.0417 (6)
C190.8796 (2)1.0287 (2)0.42266 (15)0.0387 (5)
C200.9977 (3)1.2032 (3)0.44342 (19)0.0538 (8)
H201.06241.25610.43030.065*
C210.9305 (3)1.2320 (3)0.5084 (2)0.0618 (9)
H210.95041.30510.53610.074*
N10.72834 (17)0.72638 (19)0.36341 (11)0.0314 (4)
N20.60550 (19)0.7782 (2)0.49425 (11)0.0359 (4)
N30.8395 (3)1.1603 (2)0.53250 (16)0.0566 (6)
N40.9732 (2)1.1034 (2)0.39963 (15)0.0484 (6)
N50.41189 (17)0.67804 (18)0.34940 (11)0.0299 (4)
O10.39066 (15)0.50981 (18)0.46157 (10)0.0384 (4)
O20.19162 (18)0.4762 (2)0.43227 (13)0.0607 (6)
O1W0.0413 (2)0.4789 (3)0.35398 (18)0.0851 (9)
HW120.0196 (19)0.495 (4)0.3864 (18)0.102*
HW110.1136 (19)0.461 (5)0.372 (2)0.102*
O30.4435 (2)0.9674 (3)0.19453 (16)0.0789 (8)
O40.2860 (2)0.9055 (2)0.12061 (13)0.0624 (6)
Cd10.583532 (14)0.588073 (14)0.421500 (8)0.02600 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0333 (11)0.0364 (13)0.0334 (11)0.0025 (10)0.0010 (9)0.0076 (10)
C20.0330 (11)0.0299 (11)0.0298 (11)0.0004 (9)0.0002 (9)0.0039 (9)
C30.0353 (12)0.0457 (15)0.0424 (13)0.0075 (11)0.0069 (10)0.0105 (12)
C40.0384 (12)0.0491 (15)0.0349 (12)0.0014 (11)0.0078 (10)0.0100 (11)
C50.0381 (12)0.0300 (12)0.0281 (10)0.0055 (9)0.0041 (9)0.0039 (9)
C60.0311 (11)0.0297 (11)0.0363 (12)0.0010 (9)0.0036 (9)0.0053 (9)
C70.0507 (15)0.0402 (14)0.0375 (13)0.0194 (12)0.0170 (12)0.0137 (11)
C80.0459 (14)0.0411 (14)0.0351 (12)0.0040 (11)0.0081 (11)0.0080 (11)
C90.0489 (15)0.0542 (17)0.0361 (13)0.0041 (13)0.0168 (12)0.0018 (12)
C100.0427 (14)0.0485 (16)0.0429 (14)0.0082 (12)0.0102 (12)0.0053 (12)
C110.0364 (12)0.0323 (12)0.0345 (12)0.0034 (10)0.0007 (10)0.0042 (9)
C120.0308 (10)0.0290 (11)0.0307 (11)0.0008 (9)0.0005 (9)0.0015 (9)
C130.0358 (11)0.0289 (11)0.0297 (11)0.0007 (9)0.0012 (9)0.0016 (9)
C140.0693 (19)0.0473 (17)0.0455 (15)0.0079 (15)0.0248 (14)0.0040 (13)
C150.084 (2)0.059 (2)0.0511 (18)0.0024 (17)0.0287 (18)0.0165 (15)
C160.077 (2)0.0454 (17)0.0489 (16)0.0042 (15)0.0143 (15)0.0187 (14)
C170.0475 (14)0.0328 (13)0.0384 (13)0.0003 (11)0.0015 (11)0.0056 (10)
C180.0486 (14)0.0285 (12)0.0473 (14)0.0023 (11)0.0057 (12)0.0029 (11)
C190.0404 (13)0.0309 (13)0.0439 (13)0.0045 (10)0.0060 (11)0.0062 (11)
C200.0566 (17)0.0343 (14)0.069 (2)0.0146 (13)0.0138 (15)0.0116 (14)
C210.075 (2)0.0300 (14)0.079 (2)0.0132 (14)0.0140 (18)0.0067 (15)
N10.0334 (9)0.0311 (10)0.0299 (9)0.0018 (8)0.0033 (8)0.0019 (8)
N20.0441 (11)0.0331 (11)0.0311 (10)0.0034 (9)0.0087 (9)0.0018 (8)
N30.0702 (16)0.0339 (13)0.0648 (16)0.0069 (12)0.0045 (13)0.0128 (12)
N40.0484 (13)0.0387 (13)0.0572 (15)0.0126 (10)0.0068 (11)0.0099 (11)
N50.0304 (9)0.0283 (10)0.0307 (9)0.0004 (8)0.0004 (7)0.0041 (8)
O10.0336 (8)0.0499 (11)0.0314 (8)0.0030 (8)0.0027 (7)0.0144 (8)
O20.0410 (10)0.0692 (15)0.0707 (14)0.0203 (10)0.0095 (10)0.0346 (12)
O1W0.0470 (13)0.110 (2)0.098 (2)0.0109 (15)0.0061 (13)0.0354 (19)
O30.0728 (16)0.0746 (18)0.0884 (18)0.0220 (14)0.0052 (14)0.0486 (15)
O40.0713 (14)0.0744 (17)0.0414 (11)0.0151 (12)0.0016 (10)0.0254 (10)
Cd10.02934 (9)0.02568 (9)0.02293 (9)0.00146 (6)0.00089 (6)0.00130 (6)
Geometric parameters (Å, º) top
Cd1—O1i2.2625 (16)C10—C111.403 (4)
Cd1—O12.3658 (17)C10—H100.9300
Cd1—O3ii2.372 (2)C11—C121.404 (3)
Cd1—O4ii2.520 (2)C11—C191.452 (4)
Cd1—N12.3916 (19)C12—N11.346 (3)
Cd1—N22.380 (2)C12—C131.460 (3)
Cd1—N52.3742 (19)C13—N21.349 (3)
C1—O21.227 (3)C13—C171.395 (3)
C1—O11.259 (3)C14—N21.333 (3)
C1—C21.518 (3)C14—C151.390 (4)
C2—N51.339 (3)C14—H140.9300
C2—C31.385 (3)C15—C161.352 (5)
C3—C41.384 (3)C15—H150.9300
C3—H30.9300C16—C171.399 (4)
C4—C51.384 (3)C16—H160.9300
C4—H40.9300C17—C181.453 (4)
C5—C61.385 (3)C18—N31.351 (4)
C5—C71.506 (3)C18—C191.392 (4)
C6—N51.328 (3)C19—N41.356 (3)
C6—H60.9300C20—N41.318 (4)
C7—O41.230 (4)C20—C211.389 (5)
C7—O31.241 (4)C20—H200.9300
C8—N11.331 (3)C21—N31.322 (4)
C8—C91.387 (4)C21—H210.9300
C8—H80.9300O1W—HW120.86 (3)
C9—C101.361 (4)O1W—HW110.874 (10)
C9—H90.9300
O1i—Cd1—O169.81 (7)C12—C11—C10117.5 (2)
O1i—Cd1—O3ii119.88 (10)C12—C11—C19119.8 (2)
O1—Cd1—O3ii88.73 (9)C10—C11—C19122.7 (2)
O1i—Cd1—O4ii81.48 (7)N1—C12—C11122.5 (2)
O1—Cd1—O4ii108.62 (7)N1—C12—C13117.7 (2)
O3ii—Cd1—O4ii52.55 (8)C11—C12—C13119.7 (2)
O1i—Cd1—N1126.53 (7)N2—C13—C17122.5 (2)
O1—Cd1—N1158.96 (7)N2—C13—C12117.5 (2)
O1i—Cd1—N285.52 (7)C17—C13—C12120.0 (2)
O1—Cd1—N2102.35 (7)N2—C14—C15122.7 (3)
O1i—Cd1—N5134.94 (6)N2—C14—H14118.6
O1—Cd1—N567.76 (6)C15—C14—H14118.6
O3ii—Cd1—N192.34 (9)C16—C15—C14119.0 (3)
O3ii—Cd1—N2154.57 (9)C16—C15—H15120.5
O3ii—Cd1—N573.73 (8)C14—C15—H15120.5
N1—Cd1—O4ii88.44 (7)C15—C16—C17120.1 (3)
N2—Cd1—O4ii139.53 (7)C15—C16—H16120.0
N2—Cd1—N169.21 (7)C17—C16—H16120.0
N5—Cd1—N289.21 (7)C13—C17—C16117.5 (2)
N5—Cd1—N192.38 (7)C13—C17—C18120.0 (2)
N5—Cd1—O4ii126.24 (7)C16—C17—C18122.5 (3)
O2—C1—O1124.9 (2)N3—C18—C19122.0 (3)
O2—C1—C2120.1 (2)N3—C18—C17117.9 (3)
O1—C1—C2115.0 (2)C19—C18—C17120.1 (2)
N5—C2—C3121.6 (2)N4—C19—C18121.3 (3)
N5—C2—C1116.2 (2)N4—C19—C11118.4 (2)
C3—C2—C1122.2 (2)C18—C19—C11120.3 (2)
C4—C3—C2119.2 (2)N4—C20—C21122.4 (3)
C4—C3—H3120.4N4—C20—H20118.8
C2—C3—H3120.4C21—C20—H20118.8
C3—C4—C5119.2 (2)N3—C21—C20122.9 (3)
C3—C4—H4120.4N3—C21—H21118.6
C5—C4—H4120.4C20—C21—H21118.6
C4—C5—C6117.8 (2)C8—N1—C12118.4 (2)
C4—C5—C7122.8 (2)C8—N1—Cd1124.14 (17)
C6—C5—C7119.3 (2)C12—N1—Cd1117.32 (14)
N5—C6—C5123.3 (2)C14—N2—C13118.2 (2)
N5—C6—H6118.3C14—N2—Cd1123.84 (18)
C5—C6—H6118.3C13—N2—Cd1117.77 (15)
O4—C7—O3122.7 (3)C21—N3—C18115.4 (3)
O4—C7—C5120.6 (3)C20—N4—C19115.9 (3)
O3—C7—C5116.7 (3)C6—N5—C2118.8 (2)
N1—C8—C9122.5 (2)C6—N5—Cd1122.73 (15)
N1—C8—H8118.7C2—N5—Cd1117.03 (15)
C9—C8—H8118.7C1—O1—Cd1i128.48 (15)
C10—C9—C8119.7 (2)C1—O1—Cd1121.30 (14)
C10—C9—H9120.1Cd1i—O1—Cd1110.19 (7)
C8—C9—H9120.1HW12—O1W—HW11119 (3)
C9—C10—C11119.3 (2)C7—O3—Cd1iii95.74 (19)
C9—C10—H10120.4C7—O4—Cd1iii88.98 (19)
C11—C10—H10120.4
O2—C1—C2—N5176.8 (3)C18—C19—N4—C200.8 (4)
O1—C1—C2—N52.4 (3)C11—C19—N4—C20179.4 (2)
O2—C1—C2—C32.9 (4)C5—C6—N5—C20.7 (4)
O1—C1—C2—C3177.8 (2)C5—C6—N5—Cd1165.33 (18)
N5—C2—C3—C40.2 (4)C3—C2—N5—C60.8 (4)
C1—C2—C3—C4179.5 (2)C1—C2—N5—C6178.9 (2)
C2—C3—C4—C50.5 (4)C3—C2—N5—Cd1166.0 (2)
C3—C4—C5—C60.6 (4)C1—C2—N5—Cd114.3 (3)
C3—C4—C5—C7177.4 (2)O2—C1—O1—Cd1i12.7 (4)
C4—C5—C6—N50.0 (4)C2—C1—O1—Cd1i166.54 (16)
C7—C5—C6—N5178.1 (2)O2—C1—O1—Cd1169.6 (2)
C4—C5—C7—O420.4 (4)C2—C1—O1—Cd111.1 (3)
C6—C5—C7—O4161.6 (2)O4—C7—O3—Cd1iii0.8 (3)
C4—C5—C7—O3159.1 (3)C5—C7—O3—Cd1iii179.76 (18)
C6—C5—C7—O318.9 (4)O3—C7—O4—Cd1iii0.7 (3)
N1—C8—C9—C100.1 (5)C5—C7—O4—Cd1iii179.8 (2)
C8—C9—C10—C110.7 (4)C1—O1—Cd1—O1i178.1 (2)
C9—C10—C11—C120.2 (4)Cd1i—O1—Cd1—O1i0.0
C9—C10—C11—C19179.5 (3)C1—O1—Cd1—O3ii59.3 (2)
C10—C11—C12—N10.9 (4)Cd1i—O1—Cd1—O3ii122.63 (11)
C19—C11—C12—N1178.4 (2)C1—O1—Cd1—N513.60 (19)
C10—C11—C12—C13178.9 (2)Cd1i—O1—Cd1—N5164.45 (10)
C19—C11—C12—C131.8 (3)C1—O1—Cd1—N297.6 (2)
N1—C12—C13—N20.1 (3)Cd1i—O1—Cd1—N280.47 (9)
C11—C12—C13—N2179.8 (2)C1—O1—Cd1—N133.9 (3)
N1—C12—C13—C17179.9 (2)Cd1i—O1—Cd1—N1144.18 (14)
C11—C12—C13—C170.1 (3)C1—O1—Cd1—O4ii108.8 (2)
N2—C14—C15—C160.9 (6)Cd1i—O1—Cd1—O4ii73.12 (9)
C14—C15—C16—C170.0 (6)C6—N5—Cd1—O1i158.92 (17)
N2—C13—C17—C160.6 (4)C2—N5—Cd1—O1i34.8 (2)
C12—C13—C17—C16179.5 (3)C6—N5—Cd1—O1179.7 (2)
N2—C13—C17—C18179.4 (2)C2—N5—Cd1—O114.02 (16)
C12—C13—C17—C180.6 (4)C6—N5—Cd1—O3ii84.8 (2)
C15—C16—C17—C130.7 (5)C2—N5—Cd1—O3ii81.39 (18)
C15—C16—C17—C18179.5 (3)C6—N5—Cd1—N276.04 (19)
C13—C17—C18—N3179.3 (3)C2—N5—Cd1—N2117.72 (17)
C16—C17—C18—N30.5 (4)C6—N5—Cd1—N16.89 (19)
C13—C17—C18—C190.3 (4)C2—N5—Cd1—N1173.13 (17)
C16—C17—C18—C19178.5 (3)C6—N5—Cd1—O4ii82.9 (2)
N3—C18—C19—N42.4 (4)C2—N5—Cd1—O4ii83.33 (18)
C17—C18—C19—N4176.6 (2)C14—N2—Cd1—O1i48.5 (2)
N3—C18—C19—C11179.1 (3)C13—N2—Cd1—O1i126.27 (18)
C17—C18—C19—C111.9 (4)C14—N2—Cd1—O119.7 (2)
C12—C11—C19—N4175.9 (2)C13—N2—Cd1—O1165.54 (17)
C10—C11—C19—N43.4 (4)C14—N2—Cd1—O3ii133.8 (3)
C12—C11—C19—C182.7 (4)C13—N2—Cd1—O3ii51.5 (3)
C10—C11—C19—C18178.0 (3)C14—N2—Cd1—N586.7 (2)
N4—C20—C21—N31.9 (5)C13—N2—Cd1—N598.52 (18)
C9—C8—N1—C120.9 (4)C14—N2—Cd1—N1179.6 (3)
C9—C8—N1—Cd1175.1 (2)C13—N2—Cd1—N15.68 (16)
C11—C12—N1—C81.4 (4)C14—N2—Cd1—O4ii119.8 (2)
C13—C12—N1—C8178.4 (2)C13—N2—Cd1—O4ii55.0 (2)
C11—C12—N1—Cd1174.92 (17)C8—N1—Cd1—O1i114.5 (2)
C13—C12—N1—Cd15.3 (3)C12—N1—Cd1—O1i61.66 (19)
C15—C14—N2—C131.0 (5)C8—N1—Cd1—O1108.7 (2)
C15—C14—N2—Cd1173.7 (3)C12—N1—Cd1—O175.2 (2)
C17—C13—N2—C140.3 (4)C8—N1—Cd1—O3ii16.1 (2)
C12—C13—N2—C14179.7 (2)C12—N1—Cd1—O3ii167.74 (18)
C17—C13—N2—Cd1174.76 (19)C8—N1—Cd1—N589.9 (2)
C12—C13—N2—Cd15.3 (3)C12—N1—Cd1—N593.94 (17)
C20—C21—N3—C180.4 (5)C8—N1—Cd1—N2178.2 (2)
C19—C18—N3—C211.7 (4)C12—N1—Cd1—N25.68 (16)
C17—C18—N3—C21177.3 (3)C8—N1—Cd1—O4ii36.3 (2)
C21—C20—N4—C191.3 (4)C12—N1—Cd1—O4ii139.85 (17)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y1/2, z+1/2; (iii) x+1, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—HW12···O20.86 (3)1.99 (2)2.787 (3)155 (3)
O1W—HW11···O4iv0.87 (1)1.96 (3)2.798 (3)162 (4)
Symmetry code: (iv) x, y1/2, z+1/2.
 

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