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In the ionic title compound, [Ni(H2O)6](C8H6NO5)2·5H2O, the [Co(H2O)6]2+ cation, (4-nitro­phen­oxy)acetate anions and water mol­ecules engage in O—H...O hydrogen bonding, generating a three-dimensional hydrogen-bonded network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807020041/ng2257sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807020041/ng2257Isup2.hkl
Contains datablock I

CCDC reference: 646659

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.038
  • wR factor = 0.130
  • Data-to-parameter ratio = 16.5

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.95
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 3000 Deg. PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N1 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.16
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 4 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 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

Complexes of 4-nitrophenoxyacetic acid and metal ions (M= Cu and Sn) have been structurally characterized (Prout et al., 1975; Tian et al., 2006). Recently, we reported the cobalt derivative (Gao et al., 2006); following this study, we report the nickel complex (I), which consists of a hexaaquanickel(II) cation, two 4-nitrophenoxyacetate anions and five lattice water molecules (Fig.1). The Ni(II) atom is six-coordinated in an octahedral environment. The two anions are approximately parallel. The cation, anion and lattice water molecules are linked by O—H···O hydrogen bonds into a three-dimensional network structure. (Table 1).

Related literature top

For related literature, see: Gao et al. (2006); Mirci (1990); Prout et al. (1975); Tian et al. (2006).

Experimental top

4-nitrophenoxy acetic acid was prepared by nucleophilic reaction of chloroacetic acid and 4-nitrophenol under basic conditions. (Mirci, 1990). Nickel nitrate hexahydrate (0.582 g, 2 mmol) and 4-nitrophenoxy acetic acid (0.394 g, 2 mmol) were dissolved in water and the pH was adjusted to 6 with 0.01M sodium hydroxide; green crystals separated from the filtered solution after several days.

Refinement top

H atoms bound to C atoms were placed in calculated positions and treated as riding on their parent atoms, withwith C—H = 0.93 Å (aromatic C) or C—H = 0.93 Å (methylene C), and with Uiso(H) = 1.2Ueq(C). Water H atoms were initially located in a difference Fourier map but they were treated as riding on their parent atoms with O—H = 0.85 Å and with Uiso(H) = 1.5Ueq(O).

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXL97.

Structure description top

Complexes of 4-nitrophenoxyacetic acid and metal ions (M= Cu and Sn) have been structurally characterized (Prout et al., 1975; Tian et al., 2006). Recently, we reported the cobalt derivative (Gao et al., 2006); following this study, we report the nickel complex (I), which consists of a hexaaquanickel(II) cation, two 4-nitrophenoxyacetate anions and five lattice water molecules (Fig.1). The Ni(II) atom is six-coordinated in an octahedral environment. The two anions are approximately parallel. The cation, anion and lattice water molecules are linked by O—H···O hydrogen bonds into a three-dimensional network structure. (Table 1).

For related literature, see: Gao et al. (2006); Mirci (1990); Prout et al. (1975); Tian et al. (2006).

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), showing displacement ellipsoids at the 30% probability level for non-H atoms. Dashed lines indicate the intermolecular O—H···O hydrogen bonding interactions.
Hexaaquanickel(II) bis[(4-nitrophenoxy)acetate] pentahydrate top
Crystal data top
[Ni(H2O)6](C8H6NO5)2·5H2OZ = 2
Mr = 649.14F(000) = 680
Triclinic, P1Dx = 1.586 Mg m3
Hall symbol: -p 1Mo Kα radiation, λ = 0.71073 Å
a = 7.0096 (14) ÅCell parameters from 10904 reflections
b = 10.661 (2) Åθ = 6.2–55.0°
c = 18.313 (4) ŵ = 0.81 mm1
α = 87.89 (3)°T = 293 K
β = 87.83 (3)°Block, green
γ = 84.17 (3)°0.38 × 0.21 × 0.19 mm
V = 1359.7 (5) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
5939 independent reflections
Radiation source: fine-focus sealed tube4930 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.030
ω scansθmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 98
Tmin = 0.751, Tmax = 0.864k = 1313
12966 measured reflectionsl = 2323
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)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.130H-atom parameters constrained
S = 1.14 w = 1/[σ2(Fo2) + (0.0599P)2 + 1.1083P]
where P = (Fo2 + 2Fc2)/3
5939 reflections(Δ/σ)max = 0.001
361 parametersΔρmax = 0.44 e Å3
0 restraintsΔρmin = 0.36 e Å3
Crystal data top
[Ni(H2O)6](C8H6NO5)2·5H2Oγ = 84.17 (3)°
Mr = 649.14V = 1359.7 (5) Å3
Triclinic, P1Z = 2
a = 7.0096 (14) ÅMo Kα radiation
b = 10.661 (2) ŵ = 0.81 mm1
c = 18.313 (4) ÅT = 293 K
α = 87.89 (3)°0.38 × 0.21 × 0.19 mm
β = 87.83 (3)°
Data collection top
Rigaku R-AXIS RAPID
diffractometer
5939 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
4930 reflections with I > 2σ(I)
Tmin = 0.751, Tmax = 0.864Rint = 0.030
12966 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0380 restraints
wR(F2) = 0.130H-atom parameters constrained
S = 1.14Δρmax = 0.44 e Å3
5939 reflectionsΔρmin = 0.36 e Å3
361 parameters
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
C10.3512 (4)0.7403 (3)0.02246 (15)0.0366 (6)
C20.3458 (5)0.6281 (3)0.01720 (16)0.0386 (7)
H10.32370.55490.00590.046*
C30.3733 (4)0.6255 (3)0.09147 (15)0.0351 (6)
H20.37010.55050.11890.042*
C40.4058 (4)0.7355 (3)0.12483 (14)0.0298 (5)
C50.4065 (4)0.8493 (3)0.08428 (16)0.0364 (6)
H30.42450.92340.10730.044*
C60.3803 (4)0.8511 (3)0.01020 (16)0.0388 (7)
H40.38210.92590.01750.047*
C70.4567 (4)0.6321 (2)0.24160 (14)0.0305 (6)
H50.55150.57110.21940.037*
H60.33570.59540.24670.037*
C80.5208 (4)0.6657 (2)0.31593 (14)0.0283 (5)
C90.8907 (4)0.7552 (3)0.07108 (15)0.0330 (6)
C100.8987 (4)0.6425 (3)0.11133 (17)0.0383 (6)
H70.88350.56740.08900.046*
C110.9297 (4)0.6437 (3)0.18487 (16)0.0363 (6)
H80.93510.56890.21280.044*
C120.9529 (4)0.7571 (3)0.21773 (14)0.0299 (5)
C130.9400 (4)0.8693 (3)0.17696 (15)0.0346 (6)
H90.95110.94510.19920.041*
C140.9106 (4)0.8677 (3)0.10312 (16)0.0361 (6)
H100.90430.94230.07500.043*
C151.0254 (4)0.8571 (3)0.32586 (14)0.0315 (6)
H110.90970.91530.32670.038*
H121.12590.89820.29970.038*
C161.0844 (4)0.8230 (3)0.40322 (14)0.0286 (5)
N10.3258 (5)0.7421 (3)0.10114 (15)0.0526 (7)
N20.8634 (4)0.7544 (3)0.00673 (14)0.0424 (6)
Ni10.43587 (5)0.23562 (3)0.447639 (17)0.02541 (11)
O10.5651 (3)0.57280 (19)0.35882 (11)0.0368 (5)
O20.5224 (4)0.77804 (19)0.33005 (11)0.0419 (5)
O30.4351 (3)0.74521 (19)0.19680 (11)0.0375 (5)
O40.2948 (6)0.6455 (3)0.12972 (15)0.0807 (10)
O50.3377 (6)0.8428 (3)0.13473 (15)0.0918 (12)
O61.0903 (3)0.71016 (18)0.42585 (10)0.0336 (4)
O71.1241 (3)0.91283 (19)0.43944 (11)0.0385 (5)
O80.9915 (3)0.74599 (19)0.28957 (10)0.0362 (5)
O90.8414 (5)0.6555 (3)0.03502 (14)0.0660 (8)
O100.8628 (4)0.8548 (3)0.04213 (13)0.0611 (7)
O110.4960 (3)0.32888 (18)0.34959 (10)0.0319 (4)
H130.53560.40160.35040.048*
H140.40440.34020.32020.048*
O120.6910 (3)0.11685 (18)0.43716 (10)0.0333 (4)
H150.75930.12230.39800.050*
H160.75950.10670.47470.050*
O130.3710 (3)0.14336 (18)0.54341 (10)0.0345 (4)
H170.40620.16930.58360.052*
H180.36310.06440.54830.052*
O140.1887 (3)0.3503 (2)0.46768 (11)0.0389 (5)
H190.11230.33500.50330.058*
H200.12580.37970.43100.058*
O150.2963 (3)0.1171 (2)0.38772 (11)0.0401 (5)
H210.22800.06090.40520.060*
H220.36380.08480.35230.060*
O160.5789 (3)0.36211 (17)0.49962 (10)0.0322 (4)
H230.50900.39600.53390.048*
H240.68800.33690.51650.048*
O170.9698 (3)0.4941 (2)0.36813 (13)0.0447 (5)
H250.84790.49930.37090.067*
H260.99980.56610.37930.067*
O180.8077 (4)0.1571 (3)0.29453 (13)0.0583 (7)
H270.90140.15390.26360.087*
H280.72970.22130.28470.087*
O190.2034 (4)0.3774 (2)0.25875 (15)0.0573 (6)
H290.14480.33780.22860.086*
H300.11230.40450.28780.086*
O200.4729 (4)0.0133 (2)0.26230 (13)0.0479 (6)
H310.57900.04420.25400.072*
H320.49320.06590.27030.072*
O210.1491 (4)0.1463 (2)0.20047 (13)0.0542 (6)
H330.25770.11900.21700.081*
H340.15730.13980.15430.081*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0371 (15)0.0458 (17)0.0261 (14)0.0008 (13)0.0022 (11)0.0009 (12)
C20.0471 (17)0.0356 (15)0.0338 (15)0.0044 (13)0.0062 (12)0.0046 (12)
C30.0436 (16)0.0297 (14)0.0324 (14)0.0058 (12)0.0057 (12)0.0036 (11)
C40.0302 (13)0.0332 (14)0.0254 (12)0.0012 (11)0.0030 (10)0.0015 (10)
C50.0443 (17)0.0327 (15)0.0320 (14)0.0026 (13)0.0049 (12)0.0001 (11)
C60.0429 (17)0.0404 (16)0.0324 (15)0.0034 (13)0.0029 (12)0.0088 (12)
C70.0390 (15)0.0247 (13)0.0276 (13)0.0018 (11)0.0040 (11)0.0018 (10)
C80.0308 (13)0.0267 (13)0.0273 (13)0.0036 (11)0.0001 (10)0.0013 (10)
C90.0301 (14)0.0423 (16)0.0266 (13)0.0021 (12)0.0053 (10)0.0006 (11)
C100.0417 (16)0.0354 (15)0.0393 (16)0.0088 (13)0.0080 (12)0.0035 (12)
C110.0435 (16)0.0310 (14)0.0352 (15)0.0077 (13)0.0062 (12)0.0053 (11)
C120.0275 (13)0.0353 (14)0.0267 (13)0.0023 (11)0.0026 (10)0.0016 (10)
C130.0416 (16)0.0301 (14)0.0320 (14)0.0026 (12)0.0047 (11)0.0006 (11)
C140.0406 (16)0.0348 (15)0.0320 (14)0.0001 (12)0.0062 (11)0.0057 (11)
C150.0382 (15)0.0276 (13)0.0286 (13)0.0032 (11)0.0036 (11)0.0007 (10)
C160.0273 (13)0.0319 (14)0.0263 (12)0.0033 (11)0.0001 (10)0.0012 (10)
N10.066 (2)0.062 (2)0.0296 (14)0.0051 (16)0.0069 (13)0.0001 (13)
N20.0426 (15)0.0536 (17)0.0313 (13)0.0041 (13)0.0057 (10)0.0020 (12)
Ni10.0323 (2)0.02138 (18)0.02258 (17)0.00295 (13)0.00290 (12)0.00103 (11)
O10.0508 (12)0.0290 (10)0.0304 (10)0.0026 (9)0.0093 (9)0.0054 (8)
O20.0696 (15)0.0280 (10)0.0289 (10)0.0054 (10)0.0109 (10)0.0005 (8)
O30.0586 (13)0.0275 (10)0.0267 (10)0.0044 (9)0.0091 (9)0.0023 (7)
O40.132 (3)0.076 (2)0.0369 (14)0.013 (2)0.0194 (16)0.0112 (14)
O50.164 (4)0.079 (2)0.0340 (14)0.025 (2)0.0150 (18)0.0167 (14)
O60.0386 (11)0.0306 (10)0.0319 (10)0.0053 (8)0.0062 (8)0.0043 (8)
O70.0519 (13)0.0333 (11)0.0315 (10)0.0080 (9)0.0055 (9)0.0006 (8)
O80.0515 (12)0.0317 (10)0.0262 (9)0.0066 (9)0.0075 (8)0.0026 (8)
O90.101 (2)0.0585 (17)0.0417 (14)0.0133 (15)0.0179 (14)0.0121 (12)
O100.092 (2)0.0599 (16)0.0318 (12)0.0096 (15)0.0137 (12)0.0096 (11)
O110.0417 (11)0.0256 (9)0.0287 (9)0.0056 (8)0.0046 (8)0.0033 (7)
O120.0388 (11)0.0304 (10)0.0298 (10)0.0007 (8)0.0025 (8)0.0009 (7)
O130.0523 (12)0.0269 (10)0.0255 (9)0.0094 (9)0.0052 (8)0.0033 (7)
O140.0370 (11)0.0419 (12)0.0352 (11)0.0039 (9)0.0029 (8)0.0104 (9)
O150.0539 (13)0.0366 (11)0.0329 (10)0.0183 (10)0.0034 (9)0.0038 (8)
O160.0359 (10)0.0279 (10)0.0329 (10)0.0005 (8)0.0074 (8)0.0039 (7)
O170.0460 (13)0.0330 (11)0.0542 (14)0.0022 (10)0.0104 (10)0.0004 (9)
O180.0687 (17)0.0573 (15)0.0441 (14)0.0093 (13)0.0108 (12)0.0067 (11)
O190.0625 (16)0.0543 (15)0.0564 (15)0.0053 (13)0.0182 (12)0.0036 (12)
O200.0582 (14)0.0338 (12)0.0510 (14)0.0048 (10)0.0032 (11)0.0049 (10)
O210.0668 (16)0.0596 (16)0.0365 (12)0.0064 (13)0.0066 (11)0.0021 (11)
Geometric parameters (Å, º) top
C1—C21.379 (4)C16—O71.245 (3)
C1—C61.380 (4)C16—O61.255 (3)
C1—N11.458 (4)N1—O41.214 (4)
C2—C31.380 (4)N1—O51.226 (4)
C2—H10.9300N2—O91.218 (4)
C3—C41.385 (4)N2—O101.230 (4)
C3—H20.9300Ni1—O132.038 (2)
C4—O31.351 (3)Ni1—O162.042 (2)
C4—C51.400 (4)Ni1—O142.045 (2)
C5—C61.375 (4)Ni1—O152.048 (2)
C5—H30.9300Ni1—O112.070 (2)
C6—H40.9300Ni1—O122.091 (2)
C7—O31.431 (3)O11—H130.8500
C7—C81.516 (4)O11—H140.8500
C7—H50.9700O12—H150.8499
C7—H60.9700O12—H160.8501
C8—O21.236 (3)O13—H170.8502
C8—O11.262 (3)O13—H180.8500
C9—C141.375 (4)O14—H190.8500
C9—C101.384 (4)O14—H200.8501
C9—N21.445 (4)O15—H210.8500
C10—C111.373 (4)O15—H220.8500
C10—H70.9300O16—H230.8499
C11—C121.398 (4)O16—H240.8499
C11—H80.9300O17—H250.8501
C12—O81.352 (3)O17—H260.8501
C12—C131.383 (4)O18—H270.8499
C13—C141.377 (4)O18—H280.8500
C13—H90.9300O19—H290.8500
C14—H100.9300O19—H300.8500
C15—O81.424 (3)O20—H310.8500
C15—C161.512 (4)O20—H320.8500
C15—H110.9700O21—H330.8499
C15—H120.9700O21—H340.8501
C2—C1—C6121.9 (3)H11—C15—H12108.2
C2—C1—N1119.2 (3)O7—C16—O6125.4 (3)
C6—C1—N1118.9 (3)O7—C16—C15115.2 (2)
C1—C2—C3119.4 (3)O6—C16—C15119.4 (2)
C1—C2—H1120.3O4—N1—O5123.8 (3)
C3—C2—H1120.3O4—N1—C1119.1 (3)
C2—C3—C4119.4 (3)O5—N1—C1117.2 (3)
C2—C3—H2120.3O9—N2—O10122.3 (3)
C4—C3—H2120.3O9—N2—C9119.4 (3)
O3—C4—C3125.1 (2)O10—N2—C9118.3 (3)
O3—C4—C5114.3 (2)O13—Ni1—O1692.38 (8)
C3—C4—C5120.7 (3)O13—Ni1—O1486.00 (9)
C6—C5—C4119.6 (3)O16—Ni1—O1487.80 (9)
C6—C5—H3120.2O13—Ni1—O1592.31 (9)
C4—C5—H3120.2O16—Ni1—O15175.30 (8)
C5—C6—C1119.1 (3)O14—Ni1—O1592.18 (9)
C5—C6—H4120.5O13—Ni1—O11178.78 (8)
C1—C6—H4120.5O16—Ni1—O1188.57 (8)
O3—C7—C8108.2 (2)O14—Ni1—O1193.25 (8)
O3—C7—H5110.1O15—Ni1—O1186.74 (8)
C8—C7—H5110.1O13—Ni1—O1289.70 (9)
O3—C7—H6110.1O16—Ni1—O1289.70 (8)
C8—C7—H6110.1O14—Ni1—O12174.93 (8)
H5—C7—H6108.4O15—Ni1—O1290.67 (9)
O2—C8—O1125.9 (3)O11—Ni1—O1291.09 (8)
O2—C8—C7119.0 (2)C4—O3—C7118.5 (2)
O1—C8—C7115.1 (2)C12—O8—C15117.9 (2)
C14—C9—C10121.6 (3)Ni1—O11—H13119.0
C14—C9—N2119.2 (3)Ni1—O11—H14115.7
C10—C9—N2119.1 (3)H13—O11—H14102.9
C11—C10—C9118.7 (3)Ni1—O12—H15118.6
C11—C10—H7120.6Ni1—O12—H16116.5
C9—C10—H7120.6H15—O12—H16111.7
C10—C11—C12120.1 (3)Ni1—O13—H17119.9
C10—C11—H8120.0Ni1—O13—H18124.8
C12—C11—H8120.0H17—O13—H18108.3
O8—C12—C13124.8 (3)Ni1—O14—H19121.5
O8—C12—C11114.8 (2)Ni1—O14—H20117.5
C13—C12—C11120.4 (3)H19—O14—H20110.1
C14—C13—C12119.4 (3)Ni1—O15—H21125.6
C14—C13—H9120.3Ni1—O15—H22113.9
C12—C13—H9120.3H21—O15—H22107.0
C9—C14—C13119.8 (3)Ni1—O16—H23110.7
C9—C14—H10120.1Ni1—O16—H24118.2
C13—C14—H10120.1H23—O16—H24108.2
O8—C15—C16109.7 (2)H25—O17—H26105.8
O8—C15—H11109.7H27—O18—H28109.3
C16—C15—H11109.7H29—O19—H30101.7
O8—C15—H12109.7H31—O20—H32109.7
C16—C15—H12109.7H33—O21—H34107.3
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O11—H13···O10.851.872.706 (3)167
O11—H14···O190.851.842.687 (3)176
O12—H15···O180.851.942.739 (3)156
O12—H16···O7i0.851.792.640 (3)173
O13—H17···O2ii0.851.802.652 (3)179
O13—H18···O12iii0.852.012.859 (3)173
O14—H19···O6ii0.851.972.814 (3)171
O14—H20···O17iv0.851.932.749 (3)161
O15—H21···O7v0.851.882.719 (3)168
O15—H22···O200.851.942.779 (3)169
O16—H23···O1ii0.852.042.831 (3)154
O16—H24···O6i0.851.932.762 (3)168
O17—H25···O10.852.072.885 (3)160
O17—H26···O60.851.962.789 (3)166
O18—H27···O21vi0.852.052.890 (4)173
O18—H28···O110.852.232.881 (3)133
O19—H29···O210.852.122.788 (4)135
O19—H30···O17iv0.851.972.786 (4)161
O20—H31···O180.852.263.018 (4)148
O20—H32···O2vii0.851.962.753 (3)156
O21—H33···O200.851.982.805 (4)164
O21—H34···O10viii0.852.062.905 (3)171
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+1, y+1, z+1; (iii) x+1, y, z+1; (iv) x1, y, z; (v) x1, y1, z; (vi) x+1, y, z; (vii) x, y1, z; (viii) x+1, y+1, z.

Experimental details

Crystal data
Chemical formula[Ni(H2O)6](C8H6NO5)2·5H2O
Mr649.14
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)7.0096 (14), 10.661 (2), 18.313 (4)
α, β, γ (°)87.89 (3), 87.83 (3), 84.17 (3)
V3)1359.7 (5)
Z2
Radiation typeMo Kα
µ (mm1)0.81
Crystal size (mm)0.38 × 0.21 × 0.19
Data collection
DiffractometerRigaku R-AXIS RAPID
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.751, 0.864
No. of measured, independent and
observed [I > 2σ(I)] reflections
12966, 5939, 4930
Rint0.030
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.038, 0.130, 1.14
No. of reflections5939
No. of parameters361
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.44, 0.36

Computer programs: RAPID-AUTO (Rigaku, 1998), RAPID-AUTO, CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL (Sheldrick, 1997b), SHELXL97.

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O11—H13···O10.851.872.706 (3)167.0
O11—H14···O190.851.842.687 (3)175.5
O12—H15···O180.851.942.739 (3)155.8
O12—H16···O7i0.851.792.640 (3)172.7
O13—H17···O2ii0.851.802.652 (3)178.7
O13—H18···O12iii0.852.012.859 (3)172.8
O14—H19···O6ii0.851.972.814 (3)171.0
O14—H20···O17iv0.851.932.749 (3)161.0
O15—H21···O7v0.851.882.719 (3)167.7
O15—H22···O200.851.942.779 (3)169.3
O16—H23···O1ii0.852.042.831 (3)153.8
O16—H24···O6i0.851.932.762 (3)167.9
O17—H25···O10.852.072.885 (3)159.5
O17—H26···O60.851.962.789 (3)166.4
O18—H27···O21vi0.852.052.890 (4)172.6
O18—H28···O110.852.232.881 (3)133.1
O19—H29···O210.852.122.788 (4)135.0
O19—H30···O17iv0.851.972.786 (4)161.2
O20—H31···O180.852.263.018 (4)148.2
O20—H32···O2vii0.851.962.753 (3)155.8
O21—H33···O200.851.982.805 (4)164.0
O21—H34···O10viii0.852.062.905 (3)170.5
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+1, y+1, z+1; (iii) x+1, y, z+1; (iv) x1, y, z; (v) x1, y1, z; (vi) x+1, y, z; (vii) x, y1, z; (viii) x+1, y+1, z.
 

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