Download citation
Download citation
link to html
The title compound, [Ni(C7H3NO4)(H2O)4]·2H2O, was obtained by the reaction of nickel nitrate with 2,5-pyridine­di­carboxyl­ic acid (molar ratio 1:1) in water. The compound contains a six-coordinate NiII ion, which is bonded to the N atom and an O—C group of the carboxyl­ate group in the 2-position of the 2,5-pyridine­di­carboxyl­ate ligand, and four water O atoms. Intermolecular hydrogen-bonding interactions are present, linking the nickel complex and water mol­ecules in the crystal structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803024383/bt6372sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803024383/bt6372Isup2.hkl
Contains datablock I

CCDC reference: 226682

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.028
  • wR factor = 0.054
  • Data-to-parameter ratio = 16.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.99 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - O4 = 5.46 su PLAT355_ALERT_3_C Long O-H Bond (0.82A) O10 - H10B = 1.03 Ang. PLAT417_ALERT_2_C Short Inter D-H..H-D H4A .. H9A = 2.13 Ang. PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C7 H11 N Ni O8 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 H2 O
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 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 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.

(I) top
Crystal data top
[Ni(C7H3NO4)(H2O)4]·2H2OZ = 2
Mr = 331.91F(000) = 344
Triclinic, P1Dx = 1.832 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.0177 (5) ÅCell parameters from 1951 reflections
b = 8.3138 (6) Åθ = 2.5–25°
c = 11.3906 (8) ŵ = 1.66 mm1
α = 107.128 (1)°T = 296 K
β = 99.039 (1)°Tabular, blue
γ = 102.748 (1)°0.25 × 0.10 × 0.10 mm
V = 601.60 (7) Å3
Data collection top
Bruker SMART-CCD area-detector
diffractometer
2857 independent reflections
Radiation source: fine-focus sealed tube1894 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.036
φ and ω scansθmax = 28.3°, θmin = 1.9°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1995)
h = 99
Tmin = 0.733, Tmax = 0.847k = 1011
6432 measured reflectionsl = 1515
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: difference Fourier map
wR(F2) = 0.054H-atom parameters not refined
S = 0.82 w = 1/[σ2(Fo2) + (0.0207P)2]
where P = (Fo2 + 2Fc2)/3
2857 reflections(Δ/σ)max = 0.001
172 parametersΔρmax = 0.33 e Å3
0 restraintsΔρmin = 0.35 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
Ni10.29853 (5)0.09956 (4)0.28490 (3)0.02255 (9)
O10.0884 (2)0.24173 (19)0.31830 (14)0.0313 (4)
O20.2677 (3)0.13524 (18)0.11561 (13)0.0364 (4)
O30.5141 (2)0.02726 (17)0.24019 (13)0.0264 (4)
O40.5353 (2)0.32882 (18)0.36459 (13)0.0292 (4)
O50.3134 (2)0.07225 (17)0.45736 (13)0.0253 (4)
O60.1749 (2)0.09596 (18)0.55793 (13)0.0282 (4)
O70.3715 (2)0.67513 (18)0.04316 (13)0.0309 (4)
O80.2744 (2)0.46006 (18)0.11866 (14)0.0343 (4)
O90.5834 (2)0.37772 (18)0.62690 (14)0.0365 (4)
O100.2509 (2)0.12741 (19)0.09770 (14)0.0344 (4)
N10.0810 (3)0.1366 (2)0.23546 (15)0.0202 (4)
C10.0527 (3)0.1845 (3)0.33560 (19)0.0203 (5)
C20.0890 (3)0.3346 (3)0.3258 (2)0.0259 (5)
C30.2038 (3)0.4434 (3)0.2068 (2)0.0260 (5)
C40.1725 (3)0.3986 (3)0.10192 (19)0.0216 (5)
C50.0307 (3)0.2435 (3)0.12032 (19)0.0211 (5)
C60.1910 (3)0.0606 (3)0.4613 (2)0.0212 (5)
C70.2839 (3)0.5204 (3)0.0307 (2)0.0237 (5)
H1A0.00750.22280.24400.050*
H1B0.00500.19320.36490.050*
H2A0.25990.23670.10880.050*
H2B0.25460.06240.04460.050*
H2C0.10630.35890.39950.050*
H3A0.61650.01510.30100.050*
H3B0.47250.14290.18860.050*
H3C0.31580.54430.20120.050*
H4A0.58900.33440.44640.050*
H4B0.50090.43420.37980.050*
H5A0.00060.21260.04110.050*
H9A0.49540.26370.59790.050*
H9B0.62110.39980.70710.050*
H10A0.31020.19600.05830.050*
H10B0.36060.08730.14140.050*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.02471 (17)0.02092 (16)0.01864 (16)0.00205 (12)0.00252 (12)0.00645 (11)
O10.0311 (10)0.0338 (9)0.0324 (9)0.0090 (8)0.0100 (8)0.0149 (8)
O20.0646 (13)0.0277 (9)0.0203 (9)0.0171 (9)0.0091 (8)0.0105 (7)
O30.0263 (9)0.0238 (8)0.0224 (8)0.0055 (7)0.0008 (7)0.0031 (7)
O40.0332 (10)0.0248 (8)0.0255 (9)0.0025 (7)0.0047 (7)0.0080 (7)
O50.0299 (10)0.0219 (8)0.0169 (8)0.0028 (7)0.0018 (7)0.0057 (6)
O60.0291 (10)0.0353 (9)0.0157 (8)0.0010 (7)0.0017 (7)0.0097 (7)
O70.0378 (10)0.0196 (8)0.0247 (9)0.0000 (7)0.0006 (8)0.0017 (7)
O80.0501 (12)0.0252 (9)0.0193 (9)0.0039 (8)0.0007 (8)0.0050 (7)
O90.0475 (11)0.0287 (9)0.0215 (9)0.0011 (8)0.0013 (8)0.0050 (7)
O100.0383 (10)0.0351 (10)0.0333 (10)0.0110 (8)0.0127 (8)0.0141 (8)
N10.0197 (10)0.0194 (10)0.0169 (10)0.0024 (8)0.0007 (8)0.0039 (8)
C10.0204 (12)0.0189 (11)0.0190 (12)0.0052 (9)0.0026 (10)0.0041 (9)
C20.0293 (14)0.0252 (12)0.0196 (12)0.0011 (10)0.0065 (10)0.0072 (10)
C30.0262 (14)0.0232 (12)0.0240 (13)0.0005 (10)0.0067 (11)0.0056 (10)
C40.0212 (13)0.0198 (11)0.0193 (12)0.0054 (10)0.0009 (10)0.0022 (9)
C50.0227 (13)0.0222 (12)0.0172 (11)0.0061 (10)0.0026 (10)0.0062 (9)
C60.0216 (13)0.0223 (12)0.0183 (12)0.0073 (10)0.0034 (10)0.0046 (9)
C70.0222 (13)0.0239 (13)0.0206 (12)0.0080 (10)0.0019 (10)0.0020 (10)
Geometric parameters (Å, º) top
Ni1—O12.0970 (16)C4—C71.516 (3)
Ni1—O22.0217 (15)C5—H5A1.0499
Ni1—O32.0709 (15)O1—H1A0.8913
Ni1—O52.0324 (14)O1—H1B0.9521
Ni1—O42.0801 (14)O2—H2A0.8820
Ni1—N12.0637 (16)O2—H2B0.8325
O5—C61.258 (2)O3—H3A0.8814
O6—C61.235 (2)O3—H3B0.9189
O7—C71.253 (2)O4—H4A0.9322
O8—C71.250 (3)O4—H4B0.9343
N1—C11.343 (3)O9—H9A0.9393
N1—C51.344 (2)O9—H9B0.8614
C1—C21.376 (3)O10—H10A0.9468
C1—C61.518 (3)O10—H10B1.0277
C2—C31.385 (3)C2—H2C0.9394
C3—C41.386 (3)C3—H3C0.9940
C4—C51.381 (3)
O1—Ni1—O3174.32 (6)C6—O5—Ni1116.43 (13)
O2—Ni1—O5175.81 (7)H9A—O9—H9B103.1
O4—Ni1—N1169.62 (6)H10A—O10—H10B100.5
O2—Ni1—N199.76 (7)C1—N1—C5118.10 (18)
O5—Ni1—N180.00 (6)C1—N1—Ni1112.76 (13)
O2—Ni1—O388.92 (6)C5—N1—Ni1129.14 (15)
O5—Ni1—O395.27 (6)N1—C1—C2122.96 (19)
N1—Ni1—O391.47 (6)N1—C1—C6114.74 (18)
O2—Ni1—O490.34 (6)C2—C1—C6122.3 (2)
O5—Ni1—O490.09 (6)C1—C2—C3118.4 (2)
O3—Ni1—O486.32 (6)C1—C2—H2C119.3
O2—Ni1—O186.03 (6)C3—C2—H2C122.3
O5—Ni1—O189.80 (6)C2—C3—C4119.4 (2)
N1—Ni1—O191.95 (6)C2—C3—H3C117.9
O4—Ni1—O191.10 (6)C4—C3—H3C122.4
Ni1—O1—H1A107.9C5—C4—C3118.53 (18)
Ni1—O1—H1B108.3C5—C4—C7120.3 (2)
H1A—O1—H1B105.8C3—C4—C7121.07 (19)
Ni1—O2—H2A121.1N1—C5—C4122.6 (2)
Ni1—O2—H2B128.5N1—C5—H5A118.2
H2A—O2—H2B110.3C4—C5—H5A119.0
Ni1—O3—H3A119.0O6—C6—O5125.33 (19)
Ni1—O3—H3B118.7O6—C6—C1118.67 (19)
H3A—O3—H3B107.5O5—C6—C1115.99 (19)
Ni1—O4—H4A106.6O8—C7—O7125.6 (2)
Ni1—O4—H4B116.4O8—C7—C4117.42 (19)
H4A—O4—H4B101.7O7—C7—C4116.9 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O10i0.892.082.933 (2)160
O1—H1B···O6ii0.951.832.776 (2)175
O2—H2A···O8i0.881.812.680 (2)171
O2—H2B···O100.831.892.712 (2)168
O3—H3A···O6iii0.881.842.674 (2)158
O3—H3B···O7iv0.921.792.663 (2)157
O4—H4A···O90.931.992.848 (2)153
O4—H4B···O9v0.931.812.727 (2)168
O9—H9A···O50.941.922.758 (2)147
O9—H9B···O8vi0.861.912.722 (2)157
O10—H10A···O7iv0.951.862.779 (2)164
O10—H10B···O3vii1.031.882.853 (2)158
Symmetry codes: (i) x, y, z; (ii) x, y, z+1; (iii) x+1, y, z+1; (iv) x, y1, z; (v) x+1, y+1, z+1; (vi) x+1, y+1, z+1; (vii) x+1, y, z.
 

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