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In the title compound, [Ni(C8H5O3)2(H2O)4]·4H2O the Ni atom (site symmetry \overline{1}) is coordinated by two carboxyl­ate O atoms and four water mol­ecules in an all-trans octa­hedral geometry. The coordinated and uncoordinated water mol­ecules participate in a three-dimensional network of O—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806040815/hb2162sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806040815/hb2162Isup2.hkl
Contains datablock I

CCDC reference: 627677

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.028
  • wR factor = 0.080
  • Data-to-parameter ratio = 13.9

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT417_ALERT_2_B Short Inter D-H..H-D H22 .. H31 .. 2.09 Ang.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - O1W .. 7.42 su PLAT731_ALERT_1_C Bond Calc 0.85(2), Rep 0.845(9) ...... 2.22 su-Ra O1W -H12 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(2), Rep 0.855(9) ...... 2.22 su-Ra O2W -H21 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(2), Rep 0.841(9) ...... 2.22 su-Ra O2W -H22 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.83(3), Rep 0.836(10) ...... 3.00 su-Ra O3W -H31 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(2), Rep 0.844(9) ...... 2.22 su-Ra O4W -H42 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.83(3), Rep 0.840(10) ...... 3.00 su-Ra O3W -H31 1.555 1.555 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 H2 O
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C16 H26 Ni1 O14 Atom count from _chemical_formula_moiety:C160 H108 Ni20 O684 PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 9 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 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: RAPID-AUTO (Rigaku Corporation, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
[Ni(C8H5O3)2(H2O)4]·4H2OZ = 1
Mr = 501.08F(000) = 262
Triclinic, P1Dx = 1.563 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.124 (4) ÅCell parameters from 4974 reflections
b = 7.470 (4) Åθ = 3.1–27.5°
c = 11.488 (8) ŵ = 0.98 mm1
α = 77.10 (3)°T = 293 K
β = 78.60 (3)°Prism, green
γ = 64.03 (2)°0.32 × 0.24 × 0.19 mm
V = 532.3 (6) Å3
Data collection top
Rigaku RAXIS-RAPID IP
diffractometer
2424 independent reflections
Radiation source: fine-focus sealed tube2226 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.016
ω scanθmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan
ABSCOR (Higashi, 1995)
h = 98
Tmin = 0.695, Tmax = 0.835k = 99
5303 measured reflectionsl = 1414
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) = 0.080H atoms treated by a mixture of independent and constrained refinement
S = 1.10 w = 1/[σ2(Fo2) + (0.0537P)2 + 0.0268P]
where P = (Fo2 + 2Fc2)/3
2424 reflections(Δ/σ)max = 0.001
174 parametersΔρmax = 0.34 e Å3
12 restraintsΔρmin = 0.20 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.50000.50000.50000.02825 (11)
O10.45641 (18)0.39413 (19)0.36228 (10)0.0359 (3)
O20.76977 (19)0.3173 (2)0.25347 (12)0.0485 (3)
O30.0882 (2)0.2381 (2)0.11446 (13)0.0518 (4)
O1W0.79956 (18)0.47677 (19)0.42522 (12)0.0384 (3)
O2W0.6223 (2)0.21284 (19)0.59934 (12)0.0409 (3)
O3W1.2053 (3)0.1536 (3)0.49239 (16)0.0606 (4)
O4W1.0246 (2)0.1029 (2)0.28328 (14)0.0564 (4)
C10.5820 (2)0.3395 (2)0.26978 (14)0.0301 (3)
C20.4993 (2)0.3033 (2)0.17055 (13)0.0281 (3)
C30.2926 (3)0.3236 (3)0.18304 (14)0.0345 (3)
H30.20680.35320.25470.041*
C40.2147 (3)0.3000 (3)0.08915 (15)0.0359 (3)
H40.07700.31290.09780.043*
C50.3425 (3)0.2569 (2)0.01813 (14)0.0319 (3)
C60.5488 (3)0.2357 (2)0.03069 (14)0.0338 (3)
H60.63430.20660.10250.041*
C70.6273 (3)0.2580 (2)0.06358 (15)0.0333 (3)
H70.76580.24260.05530.040*
C80.2624 (3)0.2311 (3)0.11929 (15)0.0394 (4)
H80.35070.20820.19080.047*
H110.812 (4)0.428 (3)0.3619 (13)0.057 (7)*
H120.893 (4)0.391 (3)0.4686 (19)0.085 (9)*
H210.720 (3)0.190 (4)0.6403 (19)0.072 (8)*
H220.661 (4)0.119 (3)0.559 (2)0.085 (9)*
H311.328 (3)0.145 (6)0.482 (2)0.119 (14)*
H321.159 (3)0.147 (4)0.5663 (11)0.065 (8)*
H410.967 (5)0.0243 (14)0.269 (3)0.105 (12)*
H421.001 (4)0.151 (3)0.2307 (17)0.060 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.02467 (15)0.03378 (16)0.02892 (16)0.01129 (11)0.00468 (10)0.01011 (11)
O10.0305 (6)0.0498 (7)0.0325 (6)0.0172 (5)0.0015 (4)0.0167 (5)
O20.0306 (6)0.0758 (9)0.0476 (7)0.0226 (6)0.0011 (5)0.0297 (7)
O30.0492 (8)0.0590 (8)0.0545 (8)0.0189 (7)0.0171 (6)0.0202 (7)
O1W0.0305 (6)0.0468 (7)0.0420 (7)0.0161 (5)0.0038 (5)0.0146 (6)
O2W0.0419 (7)0.0381 (6)0.0424 (7)0.0125 (5)0.0132 (5)0.0066 (5)
O3W0.0732 (11)0.0589 (9)0.0624 (10)0.0370 (9)0.0151 (8)0.0070 (8)
O4W0.0533 (8)0.0593 (9)0.0596 (9)0.0126 (7)0.0225 (7)0.0236 (8)
C10.0285 (7)0.0306 (7)0.0311 (7)0.0104 (6)0.0049 (6)0.0070 (6)
C20.0292 (7)0.0271 (7)0.0283 (7)0.0111 (6)0.0041 (6)0.0053 (5)
C30.0321 (8)0.0450 (9)0.0285 (7)0.0170 (7)0.0009 (6)0.0113 (7)
C40.0313 (8)0.0464 (9)0.0348 (8)0.0185 (7)0.0027 (6)0.0113 (7)
C50.0372 (8)0.0294 (7)0.0308 (8)0.0132 (6)0.0058 (6)0.0072 (6)
C60.0369 (8)0.0356 (8)0.0284 (7)0.0146 (7)0.0027 (6)0.0104 (6)
C70.0304 (8)0.0366 (8)0.0342 (8)0.0144 (7)0.0010 (6)0.0094 (6)
C80.0478 (10)0.0373 (8)0.0339 (8)0.0145 (8)0.0080 (7)0.0103 (7)
Geometric parameters (Å, º) top
Ni1—O12.048 (2)O4W—H410.845 (10)
Ni1—O1i2.048 (2)O4W—H420.844 (9)
Ni1—O2wi2.080 (2)C1—C21.504 (2)
Ni1—O1w2.083 (2)C2—C71.389 (2)
Ni1—O2w2.080 (2)C2—C31.394 (2)
Ni1—O1wi2.083 (2)C3—C41.382 (2)
C1—O11.263 (2)C3—H30.9300
C1—O21.254 (2)C4—C51.389 (2)
O3—C81.210 (2)C4—H40.9300
O1W—H110.859 (9)C5—C61.389 (2)
O1W—H120.845 (9)C5—C81.473 (2)
O2W—H210.855 (9)C6—C71.383 (2)
O2W—H220.841 (9)C6—H60.9300
O3W—H310.836 (10)C7—H70.9300
O3W—H320.847 (9)C8—H80.9300
O1—Ni1—O1i180.0C7—C2—C3119.75 (14)
O1—Ni1—O1w93.81 (6)C7—C2—C1119.64 (14)
O1—Ni1—O1wi86.19 (6)C3—C2—C1120.55 (14)
O1—Ni1—O2w92.37 (7)C4—C3—C2120.17 (15)
O1—Ni1—O2wi87.63 (7)C4—C3—H3119.9
O1w—Ni1—O1wi180.0C2—C3—H3119.9
O1w—Ni1—O2w91.58 (6)C3—C4—C5119.88 (15)
O1wi—Ni1—O2w88.42 (6)C3—C4—H4120.1
O2w—Ni1—O2wi180.0C5—C4—H4120.1
C1—O1—Ni1127.92 (10)C4—C5—C6120.07 (14)
Ni1—O1W—H1199.7 (16)C4—C5—C8120.71 (15)
Ni1—O1W—H12112 (2)C6—C5—C8119.22 (15)
H11—O1W—H12108.2 (14)C7—C6—C5120.05 (15)
Ni1—O2W—H21115.2 (17)C7—C6—H6120.0
Ni1—O2W—H22113.8 (19)C5—C6—H6120.0
H21—O2W—H22109.5 (15)C6—C7—C2120.06 (15)
H31—O3W—H32111.2 (16)C6—C7—H7120.0
H41—O4W—H42109.4 (15)C2—C7—H7120.0
O2—C1—O1124.73 (14)O3—C8—C5123.66 (17)
O2—C1—C2117.50 (14)O3—C8—H8118.2
O1—C1—C2117.75 (14)C5—C8—H8118.2
O2Wi—Ni1—O1—C188.22 (14)C1—C2—C3—C4176.74 (15)
O2W—Ni1—O1—C191.78 (14)C2—C3—C4—C50.4 (3)
O1Wi—Ni1—O1—C1179.96 (14)C3—C4—C5—C60.6 (2)
O1W—Ni1—O1—C10.04 (14)C3—C4—C5—C8180.00 (15)
Ni1—O1—C1—O29.4 (2)C4—C5—C6—C70.1 (2)
Ni1—O1—C1—C2169.04 (10)C8—C5—C6—C7179.54 (14)
O2—C1—C2—C73.5 (2)C5—C6—C7—C20.6 (2)
O1—C1—C2—C7175.14 (14)C3—C2—C7—C60.8 (2)
O2—C1—C2—C3179.45 (16)C1—C2—C7—C6176.29 (14)
O1—C1—C2—C32.0 (2)C4—C5—C8—O32.7 (3)
C7—C2—C3—C40.4 (2)C6—C5—C8—O3176.65 (17)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H11···O20.86 (1)1.77 (1)2.607 (2)163 (2)
O1w—H12···O3w0.85 (1)2.18 (2)2.953 (3)152 (2)
O2w—H22···O3wii0.84 (1)2.01 (1)2.819 (3)162 (3)
O2w—H21···O4wii0.86 (1)1.96 (1)2.803 (2)170 (2)
O3w—H31···O1iii0.84 (1)2.45 (3)3.037 (2)128 (3)
O3w—H32···O4wii0.85 (1)2.01 (1)2.812 (3)158 (2)
O4w—H41···O20.85 (1)2.01 (1)2.836 (3)167 (3)
O4w—H42···O3iv0.84 (1)1.92 (1)2.762 (2)173 (2)
Symmetry codes: (ii) x+2, y, z+1; (iii) x+1, y, z; (iv) x+1, y, z.
 

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