Download citation
Download citation
link to html
In the title compound, {[Cd(C15H16FN4O3)2]·3H2O}n, the CdII atom exists in a distorted octa­hedral geometry that is defined by two N atoms and four carboxyl­ate O atoms from the 1,4-dihydro-1-ethyl-6-fluoro-4-oxo-7-(piperazin-1-yl)-1,8-naphthyridine-3-carboxyl­ato monoanions. The structure is a 13.92 × 14.17 Å parallelogram grid. The Cd atom lies on a center of inversion.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806039663/ng2107sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806039663/ng2107Isup2.hkl
Contains datablock I

CCDC reference: 628010

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.004 Å
  • Disorder in solvent or counterion
  • R factor = 0.032
  • wR factor = 0.093
  • Data-to-parameter ratio = 12.0

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N2 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT411_ALERT_2_C Short Inter H...H Contact H7A .. H11 .. 2.13 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 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 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Poly[[bis(µ-1,4-dihydro-1-ethyl-6-fluoro-4-oxo-7-(piperazin-1-yl)- 1,8-naphtyridine-3-carboxylato)cadmium(II)] trihydrate] top
Crystal data top
[Cd(C15H16FN4O3)2]·3H2OF(000) = 824
Mr = 805.08Dx = 1.621 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybcCell parameters from 8360 reflections
a = 5.5628 (3) Åθ = 1.8–25.0°
b = 22.2025 (13) ŵ = 0.74 mm1
c = 13.5034 (8) ÅT = 295 K
β = 98.522 (1)°Block, colorless
V = 1649.36 (16) Å30.26 × 0.19 × 0.17 mm
Z = 2
Data collection top
Bruker SMART CCD area-detector
diffractometer
2915 independent reflections
Radiation source: fine-focus sealed tube2417 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
φ and ω scansθmax = 25.0°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 66
Tmin = 0.831, Tmax = 0.885k = 2126
8360 measured reflectionsl = 1316
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.032H-atom parameters constrained
wR(F2) = 0.093 w = 1/[σ2(Fo2) + (0.0522P)2 + 1.1028P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.007
2915 reflectionsΔρmax = 0.72 e Å3
243 parametersΔρmin = 0.46 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0029 (6)
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*/UeqOcc. (<1)
Cd10.50000.50000.50000.02468 (14)
F10.1944 (4)0.75086 (9)0.32913 (15)0.0463 (5)
C10.7412 (6)0.51767 (14)0.2951 (2)0.0336 (7)
C20.5872 (5)0.57275 (12)0.2654 (2)0.0276 (6)
C30.6371 (5)0.60252 (13)0.1819 (2)0.0310 (7)
H3A0.75510.58570.14820.037*
C40.3539 (5)0.68036 (12)0.1914 (2)0.0270 (6)
C50.0617 (5)0.76164 (13)0.2029 (2)0.0279 (6)
C60.0062 (6)0.83524 (14)0.0698 (2)0.0382 (8)
H6A0.00210.80190.02410.046*
H6B0.15120.85490.08040.046*
C70.1984 (6)0.87945 (13)0.0245 (2)0.0349 (7)
H7A0.15250.89530.03700.042*
H7B0.35100.85810.00720.042*
C80.2862 (6)0.90622 (13)0.1868 (2)0.0317 (7)
H8A0.44170.88560.17670.038*
H8B0.29800.93950.23230.038*
C90.0915 (6)0.86293 (13)0.2343 (2)0.0335 (7)
H9A0.06180.88410.25010.040*
H9B0.13570.84720.29610.040*
C100.0067 (5)0.72956 (13)0.2857 (2)0.0300 (7)
C110.1009 (5)0.67772 (13)0.3200 (2)0.0289 (6)
H110.05050.65890.37490.035*
C120.2858 (5)0.65145 (12)0.2753 (2)0.0258 (6)
C130.3988 (5)0.59572 (12)0.3161 (2)0.0254 (6)
C140.5989 (6)0.67862 (15)0.0503 (2)0.0382 (8)
H14A0.75250.66120.03910.046*
H14B0.62160.72180.05780.046*
C150.4107 (8)0.6665 (2)0.0397 (3)0.0615 (11)
H15A0.40180.62400.05260.092*
H15B0.45520.68700.09690.092*
H15C0.25530.68070.02700.092*
N10.5315 (4)0.65370 (11)0.14404 (17)0.0309 (6)
N20.2465 (5)0.73545 (13)0.1572 (2)0.0464 (7)
N30.0633 (4)0.81258 (11)0.16538 (17)0.0296 (5)
N40.2361 (4)0.93001 (10)0.09036 (17)0.0272 (5)
H40.08970.94890.10380.033*
O10.7523 (4)0.49668 (8)0.38224 (17)0.0330 (5)
O20.3261 (4)0.57352 (9)0.39234 (15)0.0319 (5)
O30.8536 (7)0.49635 (11)0.2315 (2)0.0701 (10)
O1W0.444 (3)0.5135 (5)0.0311 (7)0.163 (6)0.50
H10.40570.52480.09160.196*
O2W1.076 (4)0.4607 (7)0.0607 (11)0.299 (14)0.50
H21.09430.42610.08790.358*
O2W'1.109 (2)0.5295 (8)0.0776 (9)0.201 (7)0.50
H31.18370.55780.11180.242*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0325 (2)0.01610 (19)0.0240 (2)0.00254 (11)0.00085 (12)0.00268 (10)
F10.0528 (11)0.0400 (11)0.0526 (12)0.0166 (9)0.0293 (10)0.0147 (9)
C10.0388 (17)0.0260 (15)0.0354 (18)0.0055 (13)0.0036 (14)0.0026 (14)
C20.0337 (15)0.0209 (14)0.0271 (15)0.0032 (12)0.0010 (12)0.0022 (12)
C30.0357 (16)0.0256 (15)0.0315 (16)0.0061 (13)0.0042 (13)0.0010 (12)
C40.0319 (15)0.0222 (14)0.0265 (15)0.0028 (12)0.0033 (12)0.0041 (12)
C50.0337 (15)0.0244 (15)0.0250 (15)0.0029 (12)0.0021 (12)0.0014 (12)
C60.0496 (19)0.0330 (17)0.0338 (17)0.0165 (15)0.0126 (14)0.0099 (14)
C70.0502 (19)0.0284 (16)0.0266 (15)0.0156 (14)0.0068 (14)0.0049 (12)
C80.0417 (17)0.0267 (16)0.0269 (15)0.0067 (13)0.0057 (13)0.0017 (12)
C90.0442 (18)0.0258 (16)0.0292 (16)0.0037 (13)0.0011 (13)0.0013 (12)
C100.0366 (16)0.0257 (15)0.0292 (15)0.0051 (13)0.0097 (13)0.0035 (13)
C110.0368 (16)0.0261 (15)0.0243 (15)0.0008 (13)0.0062 (12)0.0047 (12)
C120.0304 (15)0.0207 (14)0.0255 (14)0.0019 (12)0.0011 (11)0.0030 (11)
C130.0305 (15)0.0208 (14)0.0230 (14)0.0023 (11)0.0019 (11)0.0016 (11)
C140.0434 (18)0.0376 (18)0.0369 (18)0.0088 (15)0.0171 (15)0.0151 (14)
C150.079 (3)0.074 (3)0.0334 (19)0.003 (2)0.0124 (19)0.0097 (19)
N10.0353 (13)0.0292 (13)0.0293 (13)0.0047 (11)0.0088 (10)0.0072 (10)
N20.0533 (17)0.0407 (17)0.0444 (17)0.0048 (14)0.0046 (14)0.0071 (13)
N30.0417 (14)0.0219 (12)0.0253 (12)0.0085 (11)0.0057 (10)0.0045 (10)
N40.0299 (12)0.0198 (12)0.0309 (13)0.0010 (10)0.0010 (10)0.0008 (10)
O10.0359 (12)0.0295 (12)0.0334 (13)0.0068 (8)0.0042 (10)0.0096 (9)
O20.0384 (11)0.0260 (11)0.0312 (11)0.0043 (9)0.0054 (9)0.0104 (9)
O30.106 (3)0.062 (2)0.0486 (18)0.0543 (16)0.0328 (17)0.0194 (12)
O1W0.315 (19)0.109 (9)0.066 (7)0.015 (10)0.029 (10)0.014 (6)
O2W0.62 (4)0.172 (16)0.143 (13)0.02 (2)0.181 (19)0.007 (11)
O2W'0.191 (13)0.30 (2)0.127 (10)0.066 (14)0.056 (9)0.031 (12)
Geometric parameters (Å, º) top
Cd1—O12.273 (2)C8—N41.470 (4)
Cd1—O1i2.273 (2)C8—C91.517 (4)
Cd1—O22.3015 (19)C8—H8A0.9700
Cd1—O2i2.3015 (19)C8—H8B0.9700
Cd1—N4ii2.351 (2)C9—N31.477 (4)
Cd1—N4iii2.351 (2)C9—H9A0.9700
F1—C101.357 (3)C9—H9B0.9700
C1—O31.229 (4)C10—C111.347 (4)
C1—O11.258 (4)C11—C121.395 (4)
C1—C21.513 (4)C11—H110.9300
C2—C31.371 (4)C12—C131.458 (4)
C2—C131.428 (4)C13—O21.261 (3)
C3—N11.345 (4)C14—N11.479 (4)
C3—H3A0.9300C14—C151.506 (6)
C4—N11.386 (4)C14—H14A0.9700
C4—C121.403 (4)C14—H14B0.9700
C4—N21.409 (4)C15—H15A0.9600
C5—N31.384 (4)C15—H15B0.9600
C5—N21.402 (4)C15—H15C0.9600
C5—C101.424 (4)N4—Cd1iv2.351 (2)
C6—N31.463 (4)N4—H40.9100
C6—C71.513 (4)O1W—O1Wv1.14 (2)
C6—H6A0.9700O1W—H10.8500
C6—H6B0.9700O2W—O2W'1.55 (2)
C7—N41.467 (4)O2W—H20.8519
C7—H7A0.9700O2W'—H30.8499
C7—H7B0.9700
O1—Cd1—O1i180.000 (1)N3—C9—C8110.4 (2)
O1—Cd1—O280.01 (7)N3—C9—H9A109.6
O1i—Cd1—O299.99 (7)C8—C9—H9A109.6
O1—Cd1—O2i99.99 (7)N3—C9—H9B109.6
O1i—Cd1—O2i80.01 (7)C8—C9—H9B109.6
O2—Cd1—O2i180.00 (8)H9A—C9—H9B108.1
O1—Cd1—N4ii91.06 (8)C11—C10—F1118.7 (3)
O1i—Cd1—N4ii88.94 (8)C11—C10—C5122.7 (3)
O2—Cd1—N4ii88.24 (8)F1—C10—C5118.5 (3)
O2i—Cd1—N4ii91.76 (8)C10—C11—C12121.8 (3)
O1—Cd1—N4iii88.94 (8)C10—C11—H11119.1
O1i—Cd1—N4iii91.06 (8)C12—C11—H11119.1
O2—Cd1—N4iii91.76 (8)C11—C12—C4117.6 (2)
O2i—Cd1—N4iii88.24 (8)C11—C12—C13119.7 (2)
N4ii—Cd1—N4iii180.00 (8)C4—C12—C13122.7 (2)
O3—C1—O1123.4 (3)O2—C13—C2126.8 (2)
O3—C1—C2116.9 (3)O2—C13—C12117.9 (2)
O1—C1—C2119.6 (3)C2—C13—C12115.4 (2)
C3—C2—C13118.3 (2)N1—C14—C15112.9 (3)
C3—C2—C1115.6 (3)N1—C14—H14A109.0
C13—C2—C1126.1 (2)C15—C14—H14A109.0
N1—C3—C2126.1 (3)N1—C14—H14B109.0
N1—C3—H3A116.9C15—C14—H14B109.0
C2—C3—H3A116.9H14A—C14—H14B107.8
N1—C4—C12118.3 (2)C14—C15—H15A109.5
N1—C4—N2121.1 (2)C14—C15—H15B109.5
C12—C4—N2120.6 (3)H15A—C15—H15B109.5
N3—C5—N2122.7 (3)C14—C15—H15C109.5
N3—C5—C10121.2 (3)H15A—C15—H15C109.5
N2—C5—C10115.9 (3)H15B—C15—H15C109.5
N3—C6—C7110.3 (2)C3—N1—C4119.1 (2)
N3—C6—H6A109.6C3—N1—C14119.3 (2)
C7—C6—H6A109.6C4—N1—C14121.5 (2)
N3—C6—H6B109.6C5—N2—C4121.3 (3)
C7—C6—H6B109.6C5—N3—C6116.2 (2)
H6A—C6—H6B108.1C5—N3—C9118.8 (2)
N4—C7—C6114.0 (3)C6—N3—C9110.6 (2)
N4—C7—H7A108.8C7—N4—C8109.0 (2)
C6—C7—H7A108.8C7—N4—Cd1iv108.99 (16)
N4—C7—H7B108.8C8—N4—Cd1iv120.76 (17)
C6—C7—H7B108.8C7—N4—H4105.7
H7A—C7—H7B107.6C8—N4—H4105.7
N4—C8—C9112.6 (2)Cd1iv—N4—H4105.7
N4—C8—H8A109.1C1—O1—Cd1133.8 (2)
C9—C8—H8A109.1C13—O2—Cd1129.59 (18)
N4—C8—H8B109.1O1Wv—O1W—H1153.2
C9—C8—H8B109.1O2W'—O2W—H2145.2
H8A—C8—H8B107.8O2W—O2W'—H3147.8
O3—C1—C2—C316.6 (4)C12—C4—N1—C14174.9 (3)
O1—C1—C2—C3162.2 (3)N2—C4—N1—C146.0 (4)
O3—C1—C2—C13163.5 (3)C15—C14—N1—C3102.7 (3)
O1—C1—C2—C1317.8 (5)C15—C14—N1—C474.3 (4)
C13—C2—C3—N13.0 (5)N3—C5—N2—C4173.7 (3)
C1—C2—C3—N1177.0 (3)C10—C5—N2—C40.7 (5)
N3—C6—C7—N455.7 (4)N1—C4—N2—C5178.0 (3)
N4—C8—C9—N356.9 (3)C12—C4—N2—C52.9 (4)
N3—C5—C10—C11175.6 (3)N2—C5—N3—C64.9 (4)
N2—C5—C10—C111.1 (5)C10—C5—N3—C6169.2 (3)
N3—C5—C10—F11.6 (5)N2—C5—N3—C9131.0 (3)
N2—C5—C10—F1176.1 (2)C10—C5—N3—C954.8 (4)
F1—C10—C11—C12176.4 (3)C7—C6—N3—C5164.8 (3)
C5—C10—C11—C120.9 (5)C7—C6—N3—C955.8 (3)
C10—C11—C12—C41.2 (4)C8—C9—N3—C5164.9 (3)
C10—C11—C12—C13179.2 (3)C8—C9—N3—C656.9 (3)
N1—C4—C12—C11177.8 (3)C6—C7—N4—C853.9 (3)
N2—C4—C12—C113.1 (4)C6—C7—N4—Cd1iv172.4 (2)
N1—C4—C12—C131.8 (4)C9—C8—N4—C754.2 (3)
N2—C4—C12—C13177.4 (3)C9—C8—N4—Cd1iv178.59 (18)
C3—C2—C13—O2178.5 (3)O3—C1—O1—Cd1156.1 (3)
C1—C2—C13—O21.5 (5)C2—C1—O1—Cd125.2 (4)
C3—C2—C13—C123.1 (4)O2—Cd1—O1—C113.6 (3)
C1—C2—C13—C12176.9 (3)O2i—Cd1—O1—C1166.4 (3)
C11—C12—C13—O21.0 (4)N4ii—Cd1—O1—C174.4 (3)
C4—C12—C13—O2179.4 (3)N4iii—Cd1—O1—C1105.6 (3)
C11—C12—C13—C2179.6 (3)C2—C13—O2—Cd112.8 (4)
C4—C12—C13—C20.8 (4)C12—C13—O2—Cd1165.53 (18)
C2—C3—N1—C40.2 (4)O1—Cd1—O2—C136.5 (2)
C2—C3—N1—C14177.3 (3)O1i—Cd1—O2—C13173.5 (2)
C12—C4—N1—C32.1 (4)N4ii—Cd1—O2—C1397.9 (2)
N2—C4—N1—C3177.0 (3)N4iii—Cd1—O2—C1382.1 (2)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y1/2, z+1/2; (iii) x+1, y+3/2, z+1/2; (iv) x, y+1/2, z+1/2; (v) x+1, y+1, z.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds