Penta­aqua­(pyridine-3,5-dicarboxyl­ato-κN)nickel(II) dihydrate

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.

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

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Computing details

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

Crystal data

[Ni(C7H3NO4)(H2O)5]·2H2O	F(000) = 728
Mr = 349.93	Dx = 1.805 Mg m^−3
Orthorhombic, Pna21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2n	Cell parameters from 923 reflections
a = 15.743 (1) Å	θ = 3.1–27.5°
b = 11.697 (1) Å	µ = 1.57 mm^−1
c = 6.995 (1) Å	T = 295 K
V = 1288.0 (3) Å^3	Block, green
Z = 4	0.18 × 0.09 × 0.07 mm

Data collection

Bruker SMART 1000 CCD diffractometer	2296 independent reflections
Radiation source: fine-focus sealed tube	2157 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.018
Detector resolution: 8.33 pixels mm^-1	θmax = 27.0°, θmin = 2.2°
φ and ω scans	h = −18→19
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −14→14
Tmin = 0.778, Tmax = 0.898	l = −5→8
7706 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difmap and geom
R[F^2 > 2σ(F^2)] = 0.022	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.066	w = 1/[σ^2(Fo^2) + (0.0493P)^2 + 0.0644P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = 0.001
2296 reflections	Δρmax = 0.25 e Å^−3
238 parameters	Δρmin = −0.50 e Å^−3
22 restraints	Absolute structure: Flack (1983), with 797 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.03 (1)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.82760 (1)	1.00342 (1)	0.5000 (1)	0.0201 (1)
O1	0.5493 (1)	1.2986 (1)	0.5778 (3)	0.0354 (4)
O2	0.4319 (1)	1.1991 (1)	0.5312 (4)	0.0409 (5)
O3	0.4447 (1)	0.7771 (1)	0.6070 (3)	0.0441 (5)
O4	0.5636 (1)	0.6865 (1)	0.5335 (3)	0.0304 (4)
O1w	0.9582 (1)	1.0071 (1)	0.4625 (3)	0.0293 (5)
O2w	0.8167 (1)	1.1267 (2)	0.2947 (3)	0.0303 (4)
O3w	0.8366 (1)	1.1405 (2)	0.6934 (3)	0.0283 (4)
O4w	0.8424 (1)	0.8948 (2)	0.7211 (3)	0.0391 (5)
O5w	0.8209 (1)	0.8692 (2)	0.3061 (3)	0.0278 (4)
O6w	0.2801 (1)	1.0960 (1)	0.4975 (3)	0.0376 (3)
O7w	0.2975 (1)	0.8662 (1)	0.4943 (3)	0.0403 (4)
N1	0.6945 (1)	0.9993 (1)	0.5198 (5)	0.0220 (4)
C1	0.6479 (1)	1.0960 (1)	0.5295 (3)	0.0212 (4)
C2	0.5600 (1)	1.0964 (1)	0.5465 (3)	0.0221 (4)
C3	0.5187 (1)	0.9917 (1)	0.5588 (4)	0.0236 (5)
C4	0.5653 (1)	0.8906 (1)	0.5494 (3)	0.0219 (4)
C5	0.6527 (1)	0.8987 (1)	0.5303 (3)	0.0214 (4)
C6	0.5104 (1)	1.2069 (1)	0.5533 (3)	0.0246 (5)
C7	0.5210 (1)	0.7762 (2)	0.5641 (3)	0.0253 (4)
H1w1	0.987 (1)	1.067 (1)	0.487 (6)	0.06 (1)*
H1w2	0.990 (1)	0.949 (1)	0.474 (6)	0.06 (1)*
H2w1	0.861 (1)	1.142 (3)	0.228 (4)	0.07 (1)*
H2w2	0.774 (1)	1.124 (2)	0.224 (3)	0.03 (1)*
H3w1	0.865 (1)	1.196 (2)	0.641 (3)	0.05 (1)*
H3w2	0.862 (2)	1.128 (2)	0.800 (3)	0.06 (1)*
H4w1	0.876 (1)	0.839 (2)	0.714 (4)	0.06 (1)*
H4w2	0.807 (1)	0.888 (2)	0.809 (3)	0.04 (1)*
H5w1	0.865 (1)	0.850 (3)	0.244 (4)	0.05 (1)*
H5w2	0.780 (1)	0.879 (2)	0.230 (3)	0.05 (1)*
H6w1	0.326 (1)	1.127 (2)	0.474 (5)	0.05 (1)*
H6w2	0.282 (2)	1.024 (1)	0.486 (6)	0.05 (1)*
H7w1	0.345 (1)	0.835 (2)	0.522 (4)	0.09 (1)*
H7w2	0.276 (1)	0.830 (2)	0.401 (3)	0.05 (1)*
H1	0.6761	1.1659	0.5245	0.025*
H3	0.4600	0.9891	0.5733	0.028*
H5	0.6841	0.8314	0.5244	0.026*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0152 (1)	0.0186 (1)	0.0264 (2)	0.0003 (1)	0.0012 (1)	0.0013 (1)
O1	0.027 (1)	0.020 (1)	0.059 (13)	−0.001 (1)	−0.011 (1)	−0.004 (1)
O2	0.019 (1)	0.027 (1)	0.076 (2)	0.003 (1)	−0.002 (1)	−0.008 (1)
O3	0.023 (1)	0.028 (1)	0.082 (2)	−0.005 (1)	0.009 (1)	0.005 (1)
O4	0.027 (1)	0.020 (1)	0.044 (1)	0.000 (1)	−0.004 (1)	0.002 (1)
O1w	0.018 (1)	0.025 (1)	0.045 (2)	0.001 (1)	0.001 (1)	−0.001 (1)
O2w	0.023 (1)	0.034 (1)	0.034 (1)	−0.006 (1)	−0.002 (1)	0.010 (1)
O3w	0.026 (1)	0.026 (1)	0.034 (1)	−0.004 (1)	0.000 (1)	−0.001 (1)
O4w	0.042 (1)	0.038 (1)	0.037 (1)	0.017 (1)	0.011 (1)	0.013 (1)
O5w	0.023 (1)	0.028 (1)	0.033 (1)	0.004 (1)	0.001 (1)	−0.006 (1)
O6w	0.026 (1)	0.042 (1)	0.045 (1)	−0.006 (1)	−0.002 (1)	−0.004 (1)
O7w	0.034 (1)	0.042 (1)	0.045 (1)	0.002 (1)	0.000 (1)	−0.007 (1)
N1	0.016 (1)	0.018 (1)	0.032 (1)	0.000 (1)	0.001 (1)	0.001 (1)
C1	0.018 (1)	0.017 (1)	0.028 (1)	0.000 (1)	0.000 (1)	0.001 (1)
C2	0.018 (1)	0.019 (1)	0.029 (1)	0.000 (1)	−0.001 (1)	0.000 (1)
C3	0.014 (1)	0.020 (1)	0.037 (1)	0.000 (1)	0.001 (1)	0.001 (1)
C4	0.019 (1)	0.018 (1)	0.029 (1)	−0.002 (1)	0.000 (1)	0.002 (1)
C5	0.018 (1)	0.017 (1)	0.030 (1)	0.001 (1)	0.001 (1)	0.001 (1)
C6	0.018 (1)	0.020 (1)	0.035 (1)	0.004 (1)	−0.001 (1)	−0.001 (1)
C7	0.021 (1)	0.021 (1)	0.034 (1)	−0.003 (1)	−0.003 (1)	0.003 (1)

Geometric parameters (Å, º)

Ni1—O1w	2.073 (2)	O1w—H1w1	0.85 (1)
Ni1—O2w	2.042 (2)	O1w—H1w2	0.85 (1)
Ni1—O3w	2.102 (2)	O2w—H2w1	0.85 (1)
Ni1—O4w	2.016 (2)	O2w—H2w2	0.84 (1)
Ni1—O5w	2.077 (2)	O3w—H3w1	0.86 (1)
Ni1—N1	2.101 (2)	O3w—H3w2	0.86 (1)
C6—O1	1.247 (2)	O4w—H4w1	0.84 (1)
C6—O2	1.250 (2)	O4w—H4w2	0.83 (1)
C7—O3	1.238 (2)	O5w—H5w1	0.85 (1)
C7—O4	1.263 (2)	O5w—H5w2	0.84 (1)
N1—C5	1.350 (2)	O6w—H6w1	0.83 (1)
N1—C1	1.350 (2)	O6w—H6w2	0.84 (1)
C1—C2	1.388 (2)	O7w—H7w1	0.85 (1)
C2—C3	1.389 (2)	O7w—H7w2	0.85 (1)
C2—C6	1.511 (2)	C1—H1	0.9300
C3—C4	1.394 (2)	C3—H3	0.9300
C4—C5	1.385 (2)	C5—H5	0.9300
C4—C7	1.512 (2)
O1w—Ni1—O2w	88.9 (1)	O1—C6—C2	119.1 (2)
O1w—Ni1—O3w	89.9 (1)	O2—C6—C2	116.4 (2)
O1w—Ni1—O4w	89.7 (1)	O3—C7—O4	124.2 (2)
O1w—Ni1—O5w	89.1 (1)	O3—C7—C4	117.1 (2)
O1w—Ni1—N1	176.5 (1)	O4—C7—C4	118.6 (2)
O2w—Ni1—O3w	85.4 (1)	Ni1—O1w—H1w1	122 (2)
O2w—Ni1—O4w	174.1 (1)	Ni1—O1w—H1w2	123 (2)
O2w—Ni1—O5w	94.0 (1)	H1w1—O1w—H1w2	109 (2)
O2w—Ni1—N1	88.8 (1)	Ni1—O2w—H2w1	118 (2)
O3w—Ni1—O4w	88.8 (1)	Ni1—O2w—H2w2	117 (2)
O3w—Ni1—O5w	178.9 (1)	H2w1—O2w—H2w2	110 (2)
O3w—Ni1—N1	92.4 (1)	Ni1—O3w—H3w1	109 (2)
O4w—Ni1—O5w	91.7 (1)	Ni1—O3w—H3w2	117 (2)
O4w—Ni1—N1	92.9 (1)	H3w1—O3w—H3w2	105 (1)
O5w—Ni1—N1	88.6 (1)	Ni1—O4w—H4w1	121 (2)
C5—N1—C1	117.6 (2)	Ni1—O4w—H4w2	123 (2)
C5—N1—Ni1	120.7 (1)	H4w1—O4w—H4w2	113 (2)
C1—N1—Ni1	121.7 (1)	Ni1—O5w—H5w1	120 (2)
N1—C1—C2	123.2 (2)	Ni1—O5w—H5w2	111 (2)
C1—C2—C3	118.0 (2)	H5w1—O5w—H5w2	110 (2)
C1—C2—C6	121.3 (1)	H6w1—O6w—H6w2	113 (2)
C3—C2—C6	120.6 (2)	H7w1—O7w—H7w2	108 (2)
C2—C3—C4	119.9 (2)	N1—C1—H1	118.4
C5—C4—C3	118.0 (2)	C2—C1—H1	118.4
C5—C4—C7	121.6 (2)	C2—C3—H3	120.1
C3—C4—C7	120.3 (2)	C4—C3—H3	120.1
N1—C5—C4	123.3 (2)	N1—C5—H5	118.4
O1—C6—O2	124.5 (2)	C4—C5—H5	118.4
O4w—Ni1—N1—C5	−49.3 (3)	C2—C3—C4—C5	0.8 (4)
O2w—Ni1—N1—C5	136.4 (3)	C2—C3—C4—C7	179.5 (2)
O5w—Ni1—N1—C5	42.4 (3)	C1—N1—C5—C4	0.3 (5)
O3w—Ni1—N1—C5	−138.2 (3)	Ni1—N1—C5—C4	178.0 (2)
O4w—Ni1—N1—C1	128.3 (3)	C3—C4—C5—N1	−0.2 (4)
O2w—Ni1—N1—C1	−46.0 (3)	C7—C4—C5—N1	−178.9 (3)
O5w—Ni1—N1—C1	−140.0 (3)	C1—C2—C6—O1	−12.7 (3)
O3w—Ni1—N1—C1	39.4 (3)	C3—C2—C6—O1	166.8 (2)
C5—N1—C1—C2	−1.0 (5)	C1—C2—C6—O2	166.5 (2)
Ni1—N1—C1—C2	−178.7 (2)	C3—C2—C6—O2	−14.1 (3)
N1—C1—C2—C3	1.6 (4)	C5—C4—C7—O3	170.3 (2)
N1—C1—C2—C6	−178.9 (3)	C3—C4—C7—O3	−8.3 (3)
C1—C2—C3—C4	−1.5 (4)	C5—C4—C7—O4	−9.2 (3)
C6—C2—C3—C4	179.0 (2)	C3—C4—C7—O4	172.1 (2)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H1w1···O1^i	0.85 (1)	1.96 (1)	2.807 (2)	172 (4)
O1w—H1w2···O4^ii	0.85 (1)	2.01 (1)	2.851 (2)	174 (4)
O2w—H2w1···O4^iii	0.85 (1)	1.88 (1)	2.717 (2)	165 (3)
O2w—H2w2···O7w^iv	0.84 (1)	1.96 (1)	2.766 (3)	161 (2)
O3w—H3w1···O2^i	0.86 (1)	1.80 (1)	2.657 (2)	174 (2)
O3w—H3w2···O4^v	0.86 (1)	2.12 (2)	2.902 (3)	150 (2)
O4w—H4w1···O3^ii	0.84 (1)	1.89 (1)	2.697 (2)	160 (3)
O4w—H4w2···O6w^vi	0.83 (1)	1.91 (1)	2.733 (3)	168 (2)
O5w—H5w1···O1^vii	0.85 (1)	1.88 (1)	2.722 (2)	171 (3)
O5w—H5w2···O6w^iv	0.84 (1)	1.90 (2)	2.711 (3)	160 (3)
O6w—H6w1···O2	0.83 (1)	1.91 (2)	2.687 (2)	157 (3)
O6w—H6w2···O7w	0.84 (1)	1.87 (1)	2.702 (2)	171 (4)
O7w—H7w1···O3	0.85 (1)	1.82 (1)	2.660 (2)	174 (3)
O7w—H7w2···O3w^iv	0.85 (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, z−1/2; (iv) −x+1, −y+2, z−1/2; (v) −x+3/2, y+1/2, z+1/2; (vi) −x+1, −y+2, z+1/2; (vii) −x+3/2, y−1/2, z−1/2.