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In the title compound, [Ni(C7H3NO4)(H2O)5]·2H2O, the pyridine-3,5-dicarboxyl­ate dianion bonds through its N atom to Ni, the octa­hedral geometry of the latter being completed by five water mol­ecules. Adjacent complex mol­ecules are linked through the two non-coordinated water mol­ecules, forming a three-dimensional, tightly held, hydrogen-bonded network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806008865/hb2015sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806008865/hb2015Isup2.hkl
Contains datablock I

CCDC reference: 605070

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.022
  • wR factor = 0.066
  • Data-to-parameter ratio = 9.6

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving . ? PLAT111_ALERT_2_B ADDSYM Detects (Pseudo) Centre of Symmetry ..... 90 PerFit PLAT111_ALERT_2_B ADDSYM Detects (Pseudo) Centre of Symmetry ..... 90 PerFit
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT417_ALERT_2_C Short Inter D-H..H-D H4W2 .. H6W2 .. 2.13 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 14
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.00 From the CIF: _reflns_number_total 2296 Count of symmetry unique reflns 1515 Completeness (_total/calc) 151.55% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 781 Fraction of Friedel pairs measured 0.516 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 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

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976) and SHELXTL (Bruker, 2000); software used to prepare material for publication: SHELXL97.

Pentaaqua(pyridine-3,5-dicarboxylato-κN)nickel(II) dihydrate top
Crystal data top
[Ni(C7H3NO4)(H2O)5]·2H2OF(000) = 728
Mr = 349.93Dx = 1.805 Mg m3
Orthorhombic, Pna21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2nCell parameters from 923 reflections
a = 15.743 (1) Åθ = 3.1–27.5°
b = 11.697 (1) ŵ = 1.57 mm1
c = 6.995 (1) ÅT = 295 K
V = 1288.0 (3) Å3Block, green
Z = 40.18 × 0.09 × 0.07 mm
Data collection top
Bruker SMART 1000 CCD
diffractometer
2296 independent reflections
Radiation source: fine-focus sealed tube2157 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.018
Detector resolution: 8.33 pixels mm-1θmax = 27.0°, θmin = 2.2°
φ and ω scansh = 1819
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 1414
Tmin = 0.778, Tmax = 0.898l = 58
7706 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difmap and geom
R[F2 > 2σ(F2)] = 0.022H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.066 w = 1/[σ2(Fo2) + (0.0493P)2 + 0.0644P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.001
2296 reflectionsΔρmax = 0.25 e Å3
238 parametersΔρmin = 0.50 e Å3
22 restraintsAbsolute structure: Flack (1983), with 797 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.03 (1)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.82760 (1)1.00342 (1)0.5000 (1)0.0201 (1)
O10.5493 (1)1.2986 (1)0.5778 (3)0.0354 (4)
O20.4319 (1)1.1991 (1)0.5312 (4)0.0409 (5)
O30.4447 (1)0.7771 (1)0.6070 (3)0.0441 (5)
O40.5636 (1)0.6865 (1)0.5335 (3)0.0304 (4)
O1w0.9582 (1)1.0071 (1)0.4625 (3)0.0293 (5)
O2w0.8167 (1)1.1267 (2)0.2947 (3)0.0303 (4)
O3w0.8366 (1)1.1405 (2)0.6934 (3)0.0283 (4)
O4w0.8424 (1)0.8948 (2)0.7211 (3)0.0391 (5)
O5w0.8209 (1)0.8692 (2)0.3061 (3)0.0278 (4)
O6w0.2801 (1)1.0960 (1)0.4975 (3)0.0376 (3)
O7w0.2975 (1)0.8662 (1)0.4943 (3)0.0403 (4)
N10.6945 (1)0.9993 (1)0.5198 (5)0.0220 (4)
C10.6479 (1)1.0960 (1)0.5295 (3)0.0212 (4)
C20.5600 (1)1.0964 (1)0.5465 (3)0.0221 (4)
C30.5187 (1)0.9917 (1)0.5588 (4)0.0236 (5)
C40.5653 (1)0.8906 (1)0.5494 (3)0.0219 (4)
C50.6527 (1)0.8987 (1)0.5303 (3)0.0214 (4)
C60.5104 (1)1.2069 (1)0.5533 (3)0.0246 (5)
C70.5210 (1)0.7762 (2)0.5641 (3)0.0253 (4)
H1w10.987 (1)1.067 (1)0.487 (6)0.06 (1)*
H1w20.990 (1)0.949 (1)0.474 (6)0.06 (1)*
H2w10.861 (1)1.142 (3)0.228 (4)0.07 (1)*
H2w20.774 (1)1.124 (2)0.224 (3)0.03 (1)*
H3w10.865 (1)1.196 (2)0.641 (3)0.05 (1)*
H3w20.862 (2)1.128 (2)0.800 (3)0.06 (1)*
H4w10.876 (1)0.839 (2)0.714 (4)0.06 (1)*
H4w20.807 (1)0.888 (2)0.809 (3)0.04 (1)*
H5w10.865 (1)0.850 (3)0.244 (4)0.05 (1)*
H5w20.780 (1)0.879 (2)0.230 (3)0.05 (1)*
H6w10.326 (1)1.127 (2)0.474 (5)0.05 (1)*
H6w20.282 (2)1.024 (1)0.486 (6)0.05 (1)*
H7w10.345 (1)0.835 (2)0.522 (4)0.09 (1)*
H7w20.276 (1)0.830 (2)0.401 (3)0.05 (1)*
H10.67611.16590.52450.025*
H30.46000.98910.57330.028*
H50.68410.83140.52440.026*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0152 (1)0.0186 (1)0.0264 (2)0.0003 (1)0.0012 (1)0.0013 (1)
O10.027 (1)0.020 (1)0.059 (13)0.001 (1)0.011 (1)0.004 (1)
O20.019 (1)0.027 (1)0.076 (2)0.003 (1)0.002 (1)0.008 (1)
O30.023 (1)0.028 (1)0.082 (2)0.005 (1)0.009 (1)0.005 (1)
O40.027 (1)0.020 (1)0.044 (1)0.000 (1)0.004 (1)0.002 (1)
O1w0.018 (1)0.025 (1)0.045 (2)0.001 (1)0.001 (1)0.001 (1)
O2w0.023 (1)0.034 (1)0.034 (1)0.006 (1)0.002 (1)0.010 (1)
O3w0.026 (1)0.026 (1)0.034 (1)0.004 (1)0.000 (1)0.001 (1)
O4w0.042 (1)0.038 (1)0.037 (1)0.017 (1)0.011 (1)0.013 (1)
O5w0.023 (1)0.028 (1)0.033 (1)0.004 (1)0.001 (1)0.006 (1)
O6w0.026 (1)0.042 (1)0.045 (1)0.006 (1)0.002 (1)0.004 (1)
O7w0.034 (1)0.042 (1)0.045 (1)0.002 (1)0.000 (1)0.007 (1)
N10.016 (1)0.018 (1)0.032 (1)0.000 (1)0.001 (1)0.001 (1)
C10.018 (1)0.017 (1)0.028 (1)0.000 (1)0.000 (1)0.001 (1)
C20.018 (1)0.019 (1)0.029 (1)0.000 (1)0.001 (1)0.000 (1)
C30.014 (1)0.020 (1)0.037 (1)0.000 (1)0.001 (1)0.001 (1)
C40.019 (1)0.018 (1)0.029 (1)0.002 (1)0.000 (1)0.002 (1)
C50.018 (1)0.017 (1)0.030 (1)0.001 (1)0.001 (1)0.001 (1)
C60.018 (1)0.020 (1)0.035 (1)0.004 (1)0.001 (1)0.001 (1)
C70.021 (1)0.021 (1)0.034 (1)0.003 (1)0.003 (1)0.003 (1)
Geometric parameters (Å, º) top
Ni1—O1w2.073 (2)O1w—H1w10.85 (1)
Ni1—O2w2.042 (2)O1w—H1w20.85 (1)
Ni1—O3w2.102 (2)O2w—H2w10.85 (1)
Ni1—O4w2.016 (2)O2w—H2w20.84 (1)
Ni1—O5w2.077 (2)O3w—H3w10.86 (1)
Ni1—N12.101 (2)O3w—H3w20.86 (1)
C6—O11.247 (2)O4w—H4w10.84 (1)
C6—O21.250 (2)O4w—H4w20.83 (1)
C7—O31.238 (2)O5w—H5w10.85 (1)
C7—O41.263 (2)O5w—H5w20.84 (1)
N1—C51.350 (2)O6w—H6w10.83 (1)
N1—C11.350 (2)O6w—H6w20.84 (1)
C1—C21.388 (2)O7w—H7w10.85 (1)
C2—C31.389 (2)O7w—H7w20.85 (1)
C2—C61.511 (2)C1—H10.9300
C3—C41.394 (2)C3—H30.9300
C4—C51.385 (2)C5—H50.9300
C4—C71.512 (2)
O1w—Ni1—O2w88.9 (1)O1—C6—C2119.1 (2)
O1w—Ni1—O3w89.9 (1)O2—C6—C2116.4 (2)
O1w—Ni1—O4w89.7 (1)O3—C7—O4124.2 (2)
O1w—Ni1—O5w89.1 (1)O3—C7—C4117.1 (2)
O1w—Ni1—N1176.5 (1)O4—C7—C4118.6 (2)
O2w—Ni1—O3w85.4 (1)Ni1—O1w—H1w1122 (2)
O2w—Ni1—O4w174.1 (1)Ni1—O1w—H1w2123 (2)
O2w—Ni1—O5w94.0 (1)H1w1—O1w—H1w2109 (2)
O2w—Ni1—N188.8 (1)Ni1—O2w—H2w1118 (2)
O3w—Ni1—O4w88.8 (1)Ni1—O2w—H2w2117 (2)
O3w—Ni1—O5w178.9 (1)H2w1—O2w—H2w2110 (2)
O3w—Ni1—N192.4 (1)Ni1—O3w—H3w1109 (2)
O4w—Ni1—O5w91.7 (1)Ni1—O3w—H3w2117 (2)
O4w—Ni1—N192.9 (1)H3w1—O3w—H3w2105 (1)
O5w—Ni1—N188.6 (1)Ni1—O4w—H4w1121 (2)
C5—N1—C1117.6 (2)Ni1—O4w—H4w2123 (2)
C5—N1—Ni1120.7 (1)H4w1—O4w—H4w2113 (2)
C1—N1—Ni1121.7 (1)Ni1—O5w—H5w1120 (2)
N1—C1—C2123.2 (2)Ni1—O5w—H5w2111 (2)
C1—C2—C3118.0 (2)H5w1—O5w—H5w2110 (2)
C1—C2—C6121.3 (1)H6w1—O6w—H6w2113 (2)
C3—C2—C6120.6 (2)H7w1—O7w—H7w2108 (2)
C2—C3—C4119.9 (2)N1—C1—H1118.4
C5—C4—C3118.0 (2)C2—C1—H1118.4
C5—C4—C7121.6 (2)C2—C3—H3120.1
C3—C4—C7120.3 (2)C4—C3—H3120.1
N1—C5—C4123.3 (2)N1—C5—H5118.4
O1—C6—O2124.5 (2)C4—C5—H5118.4
O4w—Ni1—N1—C549.3 (3)C2—C3—C4—C50.8 (4)
O2w—Ni1—N1—C5136.4 (3)C2—C3—C4—C7179.5 (2)
O5w—Ni1—N1—C542.4 (3)C1—N1—C5—C40.3 (5)
O3w—Ni1—N1—C5138.2 (3)Ni1—N1—C5—C4178.0 (2)
O4w—Ni1—N1—C1128.3 (3)C3—C4—C5—N10.2 (4)
O2w—Ni1—N1—C146.0 (3)C7—C4—C5—N1178.9 (3)
O5w—Ni1—N1—C1140.0 (3)C1—C2—C6—O112.7 (3)
O3w—Ni1—N1—C139.4 (3)C3—C2—C6—O1166.8 (2)
C5—N1—C1—C21.0 (5)C1—C2—C6—O2166.5 (2)
Ni1—N1—C1—C2178.7 (2)C3—C2—C6—O214.1 (3)
N1—C1—C2—C31.6 (4)C5—C4—C7—O3170.3 (2)
N1—C1—C2—C6178.9 (3)C3—C4—C7—O38.3 (3)
C1—C2—C3—C41.5 (4)C5—C4—C7—O49.2 (3)
C6—C2—C3—C4179.0 (2)C3—C4—C7—O4172.1 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O1i0.85 (1)1.96 (1)2.807 (2)172 (4)
O1w—H1w2···O4ii0.85 (1)2.01 (1)2.851 (2)174 (4)
O2w—H2w1···O4iii0.85 (1)1.88 (1)2.717 (2)165 (3)
O2w—H2w2···O7wiv0.84 (1)1.96 (1)2.766 (3)161 (2)
O3w—H3w1···O2i0.86 (1)1.80 (1)2.657 (2)174 (2)
O3w—H3w2···O4v0.86 (1)2.12 (2)2.902 (3)150 (2)
O4w—H4w1···O3ii0.84 (1)1.89 (1)2.697 (2)160 (3)
O4w—H4w2···O6wvi0.83 (1)1.91 (1)2.733 (3)168 (2)
O5w—H5w1···O1vii0.85 (1)1.88 (1)2.722 (2)171 (3)
O5w—H5w2···O6wiv0.84 (1)1.90 (2)2.711 (3)160 (3)
O6w—H6w1···O20.83 (1)1.91 (2)2.687 (2)157 (3)
O6w—H6w2···O7w0.84 (1)1.87 (1)2.702 (2)171 (4)
O7w—H7w1···O30.85 (1)1.82 (1)2.660 (2)174 (3)
O7w—H7w2···O3wiv0.85 (1)2.31 (2)2.982 (3)136 (2)
Symmetry codes: (i) x+1/2, y+5/2, z; (ii) x+1/2, y+3/2, z; (iii) x+3/2, y+1/2, z1/2; (iv) x+1, y+2, z1/2; (v) x+3/2, y+1/2, z+1/2; (vi) x+1, y+2, z+1/2; (vii) x+3/2, y1/2, z1/2.
 

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