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In the title complex, (C2H10N2)2[Cd(C7H3NO4)3]·6H2O, the CdII atom is nine-coordinated by three pyridine-2,6-di­carboxyl­ate ligands via six O atoms and three N atoms in a distorted tricapped trigonal prismatic structure. A crystallographic twofold rotation axis passes through the Cd atom and three atoms of one pyridine ring, viz. N, the C in the p-position and its attached H atom. The pyridine-2,6-di­carboxyl­ate ligands, ethyl­enedi­ammonium cations and uncoordinated water mol­ecules contribute to the formation of intermolecular hydrogen bonds, forming a three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804021567/wn6276sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804021567/wn6276Isup2.hkl
Contains datablock I

CCDC reference: 193863

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.028
  • wR factor = 0.067
  • Data-to-parameter ratio = 12.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 9 PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.15 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cd1 - O1 .. 5.75 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cd1 - O5 .. 5.43 su PLAT731_ALERT_1_C Bond Calc 0.87(3), Rep 0.867(10) ...... 3.00 su-Rat O7 -H17 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.88(3), Rep 0.876(10) ...... 3.00 su-Rat O8 -H19 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.87(3), Rep 0.867(10) ...... 3.00 su-Rat O7 -H17 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.88(3), Rep 0.876(10) ...... 3.00 su-Rat O8 -H19 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.81(3), Rep 1.804(13) ...... 2.31 su-Rat H19 -O3 1.555 3.655
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 6 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 2 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker,1997); cell refinement: SMART; data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.

Bis(ethylenediammonium) tris(pyridine-2,6-dicarboxylato-κ3O,O',N)cadmium(II) hexahydrate top
Crystal data top
(C2H10N2)2[Cd(C7H3NO4)3]·6H2ODx = 1.705 Mg m3
Mr = 840.05Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PbcnCell parameters from 5899 reflections
a = 16.250 (3) Åθ = 2.4–26.6°
b = 10.0614 (15) ŵ = 0.76 mm1
c = 20.021 (3) ÅT = 298 K
V = 3273.4 (9) Å3Block, colourless
Z = 40.40 × 0.30 × 0.15 mm
F(000) = 1728
Data collection top
Bruker SMART 1000 CCD area-detector
diffractometer
3930 independent reflections
Radiation source: fine-focus sealed tube2680 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
φ and ω scansθmax = 28.3°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 2120
Tmin = 0.751, Tmax = 0.895k = 1312
19430 measured reflectionsl = 2325
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)] = 0.028Hydrogen site location: difmap and geom
wR(F2) = 0.067H atoms treated by a mixture of independent and constrained refinement
S = 0.95 w = 1/[σ2(Fo2) + (0.035P)2]
where P = (Fo2 + 2Fc2)/3
3930 reflections(Δ/σ)max < 0.001
314 parametersΔρmax = 0.46 e Å3
6 restraintsΔρmin = 0.41 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
Cd11.00000.62545 (2)0.25000.02407 (7)
N10.88153 (10)0.74815 (16)0.21056 (8)0.0263 (4)
N21.00000.3872 (2)0.25000.0227 (5)
N30.16046 (14)0.9064 (2)0.08264 (11)0.0369 (5)
N40.09979 (14)0.6123 (2)0.04394 (12)0.0350 (5)
O11.03209 (9)0.79277 (14)0.15859 (8)0.0352 (4)
O20.97935 (10)0.92180 (18)0.07915 (8)0.0429 (4)
O30.86523 (9)0.55836 (14)0.30265 (8)0.0374 (4)
O40.73626 (10)0.61870 (15)0.32455 (9)0.0477 (5)
O50.96419 (10)0.52147 (14)0.13657 (7)0.0335 (4)
O60.98238 (10)0.33841 (16)0.07528 (8)0.0398 (4)
O70.11138 (12)0.15613 (17)0.02829 (9)0.0446 (4)
O80.17597 (11)0.35586 (19)0.11868 (9)0.0442 (4)
O90.15520 (13)0.60130 (18)0.45670 (10)0.0515 (5)
C10.97305 (14)0.8521 (2)0.13053 (11)0.0288 (5)
C20.88875 (13)0.8380 (2)0.16159 (10)0.0281 (5)
C30.82353 (15)0.9143 (2)0.13942 (13)0.0397 (6)
C40.74713 (16)0.8951 (3)0.16806 (13)0.0463 (7)
C50.73832 (15)0.8001 (3)0.21722 (13)0.0396 (6)
C60.80723 (13)0.7297 (2)0.23776 (10)0.0295 (5)
C70.80186 (13)0.6271 (2)0.29296 (11)0.0303 (5)
C80.97850 (12)0.3997 (2)0.12971 (11)0.0266 (5)
C90.99116 (12)0.3189 (2)0.19282 (10)0.0251 (4)
C100.99175 (15)0.1819 (2)0.19087 (12)0.0399 (6)
C111.00000.1132 (3)0.25000.0437 (9)
C120.15909 (17)0.8350 (2)0.01798 (12)0.0379 (6)
C130.17388 (15)0.6884 (3)0.02502 (14)0.0375 (6)
H10.8347 (14)0.974 (2)0.1046 (13)0.044 (7)*
H20.7011 (14)0.949 (2)0.1574 (12)0.042 (7)*
H30.6901 (15)0.785 (2)0.2407 (11)0.038 (7)*
H40.9864 (12)0.137 (2)0.1460 (13)0.033 (6)*
H51.00000.020 (5)0.25000.104 (19)*
H60.2156 (18)0.900 (2)0.0988 (13)0.055 (8)*
H70.1212 (17)0.869 (2)0.1088 (14)0.054 (8)*
H80.1488 (16)0.991 (3)0.0757 (13)0.056 (9)*
H90.1070 (14)0.8535 (19)0.0078 (11)0.028 (6)*
H100.2037 (16)0.868 (2)0.0078 (12)0.038 (7)*
H110.1917 (14)0.654 (2)0.0164 (12)0.032 (6)*
H120.2143 (16)0.671 (2)0.0557 (13)0.050 (7)*
H130.1095 (16)0.527 (3)0.0450 (14)0.059 (9)*
H140.0660 (18)0.626 (2)0.0137 (15)0.056 (9)*
H150.0808 (17)0.633 (2)0.0812 (14)0.050 (9)*
H160.0773 (14)0.126 (2)0.0012 (11)0.063 (10)*
H170.0838 (18)0.207 (3)0.0550 (13)0.095 (12)*
H180.1856 (17)0.2836 (19)0.1417 (13)0.074 (11)*
H190.167 (2)0.415 (3)0.1499 (13)0.097 (12)*
H200.139 (2)0.671 (2)0.4777 (14)0.083 (11)*
H210.1103 (11)0.586 (3)0.4340 (12)0.057 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.02507 (12)0.02111 (11)0.02603 (11)0.0000.00007 (9)0.000
N10.0307 (10)0.0223 (9)0.0261 (10)0.0010 (7)0.0001 (7)0.0028 (7)
N20.0208 (11)0.0239 (12)0.0235 (11)0.0000.0003 (10)0.000
N30.0320 (12)0.0304 (12)0.0484 (14)0.0046 (9)0.0045 (10)0.0007 (10)
N40.0407 (13)0.0341 (12)0.0304 (12)0.0032 (10)0.0027 (10)0.0004 (10)
O10.0308 (8)0.0366 (9)0.0381 (9)0.0004 (7)0.0003 (7)0.0087 (7)
O20.0440 (10)0.0511 (10)0.0335 (10)0.0070 (8)0.0018 (7)0.0156 (8)
O30.0283 (8)0.0345 (9)0.0494 (10)0.0016 (7)0.0034 (7)0.0124 (8)
O40.0372 (10)0.0495 (10)0.0565 (12)0.0061 (8)0.0171 (8)0.0153 (8)
O50.0424 (9)0.0269 (8)0.0311 (9)0.0019 (7)0.0047 (7)0.0008 (7)
O60.0535 (11)0.0407 (9)0.0253 (9)0.0081 (7)0.0064 (7)0.0063 (7)
O70.0588 (13)0.0344 (10)0.0407 (11)0.0004 (9)0.0073 (9)0.0066 (8)
O80.0397 (10)0.0481 (12)0.0447 (11)0.0034 (8)0.0017 (8)0.0149 (10)
O90.0584 (13)0.0413 (11)0.0547 (13)0.0043 (10)0.0186 (10)0.0066 (9)
C10.0356 (12)0.0229 (11)0.0278 (12)0.0063 (9)0.0031 (9)0.0050 (9)
C20.0324 (12)0.0277 (11)0.0243 (11)0.0015 (9)0.0009 (9)0.0001 (9)
C30.0440 (15)0.0400 (14)0.0350 (14)0.0078 (11)0.0009 (11)0.0089 (11)
C40.0400 (15)0.0586 (18)0.0404 (15)0.0197 (12)0.0035 (11)0.0071 (13)
C50.0321 (14)0.0517 (16)0.0350 (14)0.0070 (11)0.0016 (11)0.0040 (13)
C60.0285 (12)0.0283 (11)0.0317 (14)0.0013 (9)0.0005 (9)0.0012 (9)
C70.0305 (12)0.0278 (11)0.0325 (12)0.0037 (10)0.0004 (9)0.0019 (10)
C80.0231 (11)0.0330 (13)0.0238 (11)0.0019 (8)0.0016 (8)0.0003 (9)
C90.0263 (11)0.0230 (10)0.0260 (11)0.0018 (8)0.0002 (8)0.0014 (8)
C100.0630 (18)0.0263 (11)0.0304 (13)0.0028 (11)0.0046 (11)0.0029 (10)
C110.077 (3)0.0185 (15)0.0361 (18)0.0000.0011 (18)0.000
C120.0343 (14)0.0433 (14)0.0362 (14)0.0066 (11)0.0016 (11)0.0051 (11)
C130.0321 (14)0.0417 (14)0.0386 (15)0.0007 (11)0.0007 (11)0.0059 (12)
Geometric parameters (Å, º) top
Cd1—N22.397 (2)O7—H160.864 (10)
Cd1—N1i2.4194 (17)O7—H170.867 (10)
Cd1—N12.4194 (17)O8—H180.874 (10)
Cd1—O32.5225 (15)O8—H190.876 (10)
Cd1—O3i2.5225 (15)O9—H200.861 (10)
Cd1—O1i2.5408 (15)O9—H210.872 (10)
Cd1—O12.5408 (15)C1—C21.511 (3)
Cd1—O52.5671 (15)C2—C31.382 (3)
Cd1—O5i2.5671 (15)C3—C41.381 (3)
N1—C61.337 (3)C3—H10.94 (2)
N1—C21.339 (3)C4—C51.379 (4)
N2—C9i1.343 (2)C4—H20.95 (2)
N2—C91.343 (2)C5—C61.387 (3)
N3—C121.481 (3)C5—H30.93 (2)
N3—H60.95 (3)C6—C71.515 (3)
N3—H70.91 (3)C8—C91.516 (3)
N3—H80.88 (3)C9—C101.380 (3)
N4—C131.476 (3)C10—C111.377 (3)
N4—H130.88 (3)C10—H41.01 (2)
N4—H140.83 (3)C11—C10i1.377 (3)
N4—H150.83 (3)C11—H50.94 (5)
O1—C11.262 (3)C12—C131.501 (3)
O2—C11.249 (3)C12—H91.01 (2)
O3—C71.255 (2)C12—H100.95 (2)
O4—C71.242 (3)C13—H110.94 (2)
O5—C81.255 (2)C13—H120.92 (3)
O6—C81.254 (3)
N2—Cd1—N1i120.68 (4)H14—N4—H15112 (3)
N2—Cd1—N1120.68 (4)C1—O1—Cd1118.54 (14)
N1i—Cd1—N1118.64 (8)C7—O3—Cd1120.02 (13)
N2—Cd1—O374.48 (3)C8—O5—Cd1116.93 (13)
N1i—Cd1—O3133.71 (5)H16—O7—H17107 (3)
N1—Cd1—O365.30 (5)H18—O8—H19103 (3)
N2—Cd1—O3i74.48 (3)H20—O9—H2198 (3)
N1i—Cd1—O3i65.30 (5)O2—C1—O1124.7 (2)
N1—Cd1—O3i133.71 (5)O2—C1—C2117.8 (2)
O3—Cd1—O3i148.95 (7)O1—C1—C2117.5 (2)
N2—Cd1—O1i131.50 (3)N1—C2—C3122.9 (2)
N1i—Cd1—O1i65.81 (5)N1—C2—C1116.37 (18)
N1—Cd1—O1i74.55 (5)C3—C2—C1120.7 (2)
O3—Cd1—O1i72.43 (5)C4—C3—C2118.6 (2)
O3i—Cd1—O1i131.04 (5)C4—C3—H1124.8 (14)
N2—Cd1—O1131.50 (3)C2—C3—H1116.6 (14)
N1i—Cd1—O174.55 (5)C5—C4—C3119.1 (2)
N1—Cd1—O165.81 (5)C5—C4—H2118.4 (14)
O3—Cd1—O1131.04 (5)C3—C4—H2122.3 (14)
O3i—Cd1—O172.43 (5)C4—C5—C6118.8 (2)
O1i—Cd1—O197.01 (7)C4—C5—H3124.2 (15)
N2—Cd1—O565.95 (3)C6—C5—H3116.7 (15)
N1i—Cd1—O5132.61 (5)N1—C6—C5122.5 (2)
N1—Cd1—O574.86 (5)N1—C6—C7116.33 (18)
O3—Cd1—O593.66 (5)C5—C6—C7121.2 (2)
O3i—Cd1—O573.62 (5)O4—C7—O3126.0 (2)
O1i—Cd1—O5149.40 (5)O4—C7—C6117.84 (19)
O1—Cd1—O571.30 (5)O3—C7—C6116.15 (19)
N2—Cd1—O5i65.95 (3)O6—C8—O5125.8 (2)
N1i—Cd1—O5i74.86 (5)O6—C8—C9117.00 (19)
N1—Cd1—O5i132.61 (5)O5—C8—C9117.21 (19)
O3—Cd1—O5i73.62 (5)N2—C9—C10122.3 (2)
O3i—Cd1—O5i93.66 (5)N2—C9—C8116.79 (18)
O1i—Cd1—O5i71.30 (5)C10—C9—C8120.9 (2)
O1—Cd1—O5i149.40 (5)C11—C10—C9118.5 (2)
O5—Cd1—O5i131.90 (6)C11—C10—H4123.3 (12)
C6—N1—C2118.10 (18)C9—C10—H4118.1 (13)
C6—N1—Cd1120.98 (14)C10i—C11—C10119.8 (3)
C2—N1—Cd1120.92 (13)C10i—C11—H5120.09 (15)
C9i—N2—C9118.5 (2)C10—C11—H5120.09 (15)
C9i—N2—Cd1120.77 (12)N3—C12—C13113.1 (2)
C9—N2—Cd1120.77 (12)N3—C12—H9111.7 (12)
C12—N3—H6106.0 (16)C13—C12—H9111.4 (11)
C12—N3—H7107.0 (16)N3—C12—H10107.1 (14)
H6—N3—H7116 (2)C13—C12—H10105.7 (13)
C12—N3—H8109.0 (18)H9—C12—H10107.3 (19)
H6—N3—H8109 (2)N4—C13—C12113.8 (2)
H7—N3—H8110 (2)N4—C13—H11106.5 (13)
C13—N4—H13111.6 (18)C12—C13—H11109.3 (13)
C13—N4—H14105.2 (19)N4—C13—H12108.3 (16)
H13—N4—H14108 (2)C12—C13—H12111.4 (15)
C13—N4—H15113.9 (18)H11—C13—H12107 (2)
H13—N4—H15107 (2)
N3—C12—C13—N481.9 (3)
Symmetry code: (i) x+2, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N3—H6···O8ii0.95 (3)1.86 (3)2.801 (3)168 (2)
N3—H7···O1iii0.91 (3)1.92 (3)2.823 (3)176 (2)
N3—H8···O7iv0.88 (3)2.01 (3)2.852 (3)160 (2)
N4—H13···O9v0.88 (3)2.31 (3)2.912 (3)126 (2)
N4—H14···O6vi0.83 (3)1.98 (3)2.779 (3)162 (3)
N4—H15···O1iii0.83 (3)2.37 (3)3.126 (3)151 (2)
O7—H16···O2vi0.86 (1)1.88 (1)2.723 (3)167 (3)
O7—H17···O6iii0.87 (1)2.15 (2)2.940 (2)151 (3)
O8—H18···O4vii0.87 (1)1.97 (1)2.819 (2)163 (3)
O8—H19···O3viii0.88 (1)1.80 (1)2.661 (2)165 (3)
O9—H20···O7ix0.86 (1)2.06 (1)2.919 (3)175 (3)
O9—H21···O5viii0.87 (1)1.97 (1)2.810 (2)161 (3)
Symmetry codes: (ii) x+1/2, y+1/2, z; (iii) x1, y, z; (iv) x, y+1, z; (v) x, y+1, z1/2; (vi) x+1, y+1, z; (vii) x1/2, y1/2, z+1/2; (viii) x+1, y, z+1/2; (ix) x, y+1, z+1/2.
 

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