Potassium tris­(acetyl­acetonato)­nickelate(II) 0.3-hydrate

Atencio, R.; Reyes, J.; Ramírez, K.; González, T.; Alvarado, Y.

doi:10.1107/S1600536804013017

Potassium tris(acetylacetonato)nickelate(II) 0.3-hydrate

R. Atencio, J. Reyes, K. Ramírez, T. González and Y. Alvarado

The crystal structure of the title compound, K[Ni(C₅H₇O₂)₃]·0.3H₂O, comprises a columnar array with K

O interactions between the K⁺ ions and the O atoms on opposite faces of the NiO₆ octahedron of the complex anion. The columns are maintained, almost exclusively, by hydrophobic methyl–methyl interactions.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804013017/ob6375sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536804013017/ob6375Isup2.hkl Contains datablock I

CCDC reference: 245113

checkCIF report

Key indicators

Single-crystal X-ray study
T = 298 K
H-atom completeness 98%
R factor = 0.027
wR factor = 0.079
Data-to-parameter ratio = 8.3

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......       0.94

Alert level B
PLAT027_ALERT_3_B _diffrn_reflns_theta_full (too) Low ............      24.96 Deg.

Alert level C
REFLT03_ALERT_1_C  Reflection count < 95% complete
           From the CIF: _diffrn_reflns_theta_max           24.96
           From the CIF: _diffrn_reflns_theta_full           0.00
           From the CIF: _reflns_number_total               1744
           TEST2: Reflns within _diffrn_reflns_theta_max
           Count of symmetry unique reflns         1861
           Completeness (_total/calc)             93.71%
PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low ....       0.94
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms .....          1
PLAT301_ALERT_3_C Main Residue  Disorder .........................       1.00 Perc.
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          7
PLAT380_ALERT_4_C Incorrectly Oriented X(sp2)-Methyl Moiety ......        C14
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.19 Ratio

Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C15 H21.6 K1 Ni1 O6.3
            Atom count from the _atom_site data:  C15 H21 K1 Ni1 O6.3
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    4
           From the CIF: _chemical_formula_sum  C15 H21.6 K Ni O6.3
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C         60.00     60.00    0.00
           H         86.40     84.00    2.40
           K          4.00      4.00    0.00
           Ni         4.00      4.00    0.00
           O         25.20     25.20    0.00
REFLT03_ALERT_4_G  WARNING: Large fraction of Friedel related reflns may
                     be needed to determine absolute structure
           From the CIF: _diffrn_reflns_theta_max           24.96
           From the CIF: _reflns_number_total               1744
           Count of symmetry unique reflns         1861
           Completeness (_total/calc)             93.71%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured         0
           Fraction of Friedel pairs measured     0.000
           Are heavy atom types Z>Si present        yes

   1 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
  10 ALERT level C = Check and explain
   4 ALERT level G = General alerts; check

   6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   6 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SHELXTL-NT (Bruker, 1998); program(s) used to refine structure: SHELXTL-NT; molecular graphics: SHELXTL-NT and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXTL-NT.

(I) top

Crystal data top

K[Ni(C₅H₇O₂)₃]·0.3H₂O	F(000) = 836
M_r = 400.53	D_x = 1.303 Mg m⁻³
Orthorhombic, Pna2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2n	Cell parameters from 10 reflections
a = 13.272 (3) Å	θ = 23.3–31.0°
b = 9.905 (2) Å	µ = 1.18 mm⁻¹
c = 15.533 (3) Å	T = 298 K
V = 2042.0 (7) Å³	Needle, pale green
Z = 4	0.42 × 0.22 × 0.20 mm

Data collection top

Rigaku AFC7S diffractometer	1582 reflections with I > 2σ(I)
Radiation source: Normal-focus sealed tube	R_int = 0.006
Graphite monochromator	θ_max = 25.0°, θ_min = 2.6°
ω–2θ scans	h = 0→15
Absorption correction: psi scan (North et al., 1968)	k = −11→2
T_min = 0.638, T_max = 0.799	l = −1→17
1789 measured reflections	3 standard reflections every 150 reflections
1744 independent reflections	intensity decay: none

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.028	H-atom parameters constrained
wR(F²) = 0.079	w = 1/[σ²(F_o²) + (0.0519P)² + 0.3003P] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max < 0.001
1744 reflections	Δρ_max = 0.16 e Å⁻³
209 parameters	Δρ_min = −0.18 e Å⁻³
1 restraint	Absolute structure: Flack (1983), 1 Friedel pair
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.05 (3)

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. The coordinates of a centrosymmetrical model were also refined, which yielded to larger final R-factors in comparison with the original model.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ni1	0.25114 (3)	0.23367 (4)	0.22656 (8)	0.05069 (16)
K1	0.50360 (5)	0.17937 (10)	0.22630 (15)	0.0754 (3)
O3	0.33998 (19)	0.2025 (3)	0.3395 (2)	0.0620 (8)
O6	0.16423 (19)	0.2633 (3)	0.1134 (2)	0.0657 (9)
O1	0.32063 (19)	0.0674 (3)	0.1746 (2)	0.0641 (8)
O2	0.13588 (18)	0.1208 (3)	0.2776 (2)	0.0611 (7)
O4	0.18795 (19)	0.3979 (3)	0.2900 (2)	0.0683 (8)
O5	0.36043 (18)	0.3504 (3)	0.1705 (2)	0.0617 (8)
C12	0.2787 (4)	0.3987 (6)	0.0290 (4)	0.0637 (12)
H12A	0.2880	0.4421	−0.0234	0.076*
C7	0.2814 (4)	0.3879 (6)	0.4267 (4)	0.0730 (14)
H7A	0.2900	0.4324	0.4790	0.088*
C11	0.3571 (3)	0.4086 (4)	0.0927 (3)	0.0577 (11)
C3	0.1284 (3)	−0.0061 (4)	0.2691 (3)	0.0569 (10)
C15	0.1158 (4)	0.3229 (7)	−0.0373 (4)	0.0951 (18)
H15A	0.0567	0.2721	−0.0223	0.143*
H15B	0.1489	0.2806	−0.0852	0.143*
H15C	0.0966	0.4131	−0.0528	0.143*
C10	0.1567 (4)	0.5687 (6)	0.3986 (5)	0.108 (2)
H10A	0.1119	0.5981	0.3538	0.161*
H10B	0.2047	0.6387	0.4107	0.161*
H10C	0.1186	0.5492	0.4496	0.161*
C1	0.2889 (3)	−0.0524 (5)	0.1869 (3)	0.0628 (11)
C13	0.1897 (3)	0.3275 (5)	0.0420 (3)	0.0615 (11)
C2	0.1983 (3)	−0.0899 (4)	0.2275 (4)	0.0700 (10)
H2A	0.1830	−0.1815	0.2267	0.084*
C9	0.4079 (5)	0.2233 (6)	0.4876 (5)	0.103 (2)
H9A	0.4442	0.1440	0.4702	0.155*
H9B	0.3668	0.2026	0.5367	0.155*
H9C	0.4548	0.2934	0.5022	0.155*
C6	0.3396 (3)	0.2717 (4)	0.4121 (3)	0.0648 (12)
C14	0.4474 (4)	0.4927 (5)	0.0687 (3)	0.0757 (13)
H14A	0.4948	0.4925	0.1154	0.114*
H14B	0.4263	0.5837	0.0573	0.114*
H14C	0.4786	0.4557	0.0182	0.114*
C8	0.2123 (3)	0.4414 (5)	0.3693 (4)	0.0684 (13)
C5	0.0335 (4)	−0.0685 (5)	0.3082 (4)	0.0811 (14)
H5A	−0.0070	0.0013	0.3337	0.122*
H5B	0.0522	−0.1328	0.3516	0.122*
H5C	−0.0044	−0.1131	0.2639	0.122*
C4	0.3588 (4)	−0.1622 (6)	0.1521 (5)	0.1000 (19)
H4A	0.4167	−0.1211	0.1260	0.150*
H4B	0.3235	−0.2150	0.1099	0.150*
H4C	0.3800	−0.2195	0.1985	0.150*
O1W	0.6063 (4)	−0.0740 (6)	0.1814 (5)	0.149 (7)*	0.30

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0288 (2)	0.0535 (3)	0.0698 (3)	−0.00048 (16)	0.0000 (2)	−0.0045 (4)
K1	0.0291 (3)	0.0831 (6)	0.1140 (7)	0.0000 (3)	−0.0017 (5)	0.0033 (11)
O3	0.0440 (14)	0.0633 (17)	0.079 (2)	0.0016 (13)	−0.0057 (15)	−0.0075 (17)
O6	0.0361 (15)	0.079 (2)	0.082 (2)	−0.0022 (13)	−0.0087 (15)	−0.0021 (17)
O1	0.0427 (14)	0.0646 (18)	0.085 (2)	0.0041 (13)	0.0041 (14)	−0.0154 (16)
O2	0.0379 (13)	0.0623 (16)	0.083 (2)	−0.0045 (12)	0.0027 (13)	−0.0049 (15)
O4	0.0406 (14)	0.0591 (16)	0.105 (3)	0.0039 (13)	0.0034 (16)	−0.0120 (17)
O5	0.0362 (13)	0.0668 (17)	0.082 (2)	−0.0085 (12)	−0.0002 (14)	0.0042 (16)
C12	0.059 (2)	0.065 (3)	0.068 (3)	−0.004 (3)	0.002 (2)	0.000 (3)
C7	0.073 (3)	0.068 (3)	0.078 (4)	−0.010 (3)	0.003 (3)	−0.020 (3)
C11	0.047 (2)	0.052 (2)	0.075 (3)	0.0027 (17)	0.0086 (19)	−0.008 (2)
C3	0.052 (2)	0.062 (2)	0.057 (2)	−0.0086 (19)	−0.0111 (18)	0.007 (2)
C15	0.070 (3)	0.114 (5)	0.102 (4)	−0.010 (3)	−0.031 (3)	0.007 (4)
C10	0.091 (4)	0.073 (3)	0.159 (6)	0.017 (3)	0.015 (4)	−0.035 (4)
C1	0.067 (3)	0.061 (2)	0.061 (2)	0.012 (2)	−0.005 (2)	−0.011 (2)
C13	0.055 (2)	0.062 (2)	0.068 (3)	0.010 (2)	−0.008 (2)	−0.007 (2)
C2	0.076 (3)	0.0521 (19)	0.082 (3)	−0.0003 (19)	−0.006 (3)	0.000 (3)
C9	0.115 (5)	0.089 (4)	0.105 (5)	−0.010 (3)	−0.045 (4)	−0.004 (3)
C6	0.056 (2)	0.062 (3)	0.076 (3)	−0.018 (2)	−0.007 (2)	−0.004 (2)
C14	0.064 (3)	0.078 (3)	0.085 (3)	−0.020 (2)	0.010 (2)	−0.005 (3)
C8	0.054 (2)	0.054 (2)	0.097 (4)	−0.012 (2)	0.014 (3)	−0.020 (2)
C5	0.078 (3)	0.080 (3)	0.084 (3)	−0.029 (3)	0.007 (3)	0.008 (3)
C4	0.090 (4)	0.076 (3)	0.134 (5)	0.032 (3)	0.008 (4)	−0.014 (4)

Geometric parameters (Å, º) top

Ni1—O5	2.049 (3)	C7—C6	1.404 (7)
Ni1—O1	2.053 (3)	C7—H7A	0.9300
Ni1—O2	2.054 (3)	C11—C14	1.506 (6)
Ni1—O4	2.079 (3)	C3—C2	1.402 (6)
Ni1—O6	2.123 (3)	C3—C5	1.529 (6)
Ni1—O3	2.137 (3)	C15—C13	1.576 (7)
Ni1—K1	3.3936 (11)	C15—H15A	0.9600
Ni1—K1ⁱ	3.3963 (10)	C15—H15B	0.9600
K1—O5	2.689 (3)	C15—H15C	0.9600
K1—O4ⁱⁱ	2.748 (3)	C10—C8	1.530 (7)
K1—O2ⁱⁱ	2.763 (3)	C10—H10A	0.9600
K1—O1	2.788 (3)	C10—H10B	0.9600
K1—O3	2.804 (3)	C10—H10C	0.9600
K1—O6ⁱⁱ	2.819 (4)	C1—C2	1.409 (7)
K1—O1W	2.940 (5)	C1—C4	1.528 (6)
K1—Ni1ⁱⁱ	3.3963 (10)	C2—H2A	0.9300
O3—C6	1.320 (6)	C9—C6	1.557 (8)
O6—C13	1.323 (6)	C9—H9A	0.9600
O6—K1ⁱ	2.819 (4)	C9—H9B	0.9600
O1—C1	1.273 (6)	C9—H9C	0.9600
O2—C3	1.268 (5)	C14—H14A	0.9600
O2—K1ⁱ	2.763 (3)	C14—H14B	0.9600
O4—C8	1.344 (6)	C14—H14C	0.9600
O4—K1ⁱ	2.748 (3)	C5—H5A	0.9600
O5—C11	1.340 (5)	C5—H5B	0.9600
C12—C13	1.390 (7)	C5—H5C	0.9600
C12—C11	1.439 (7)	C4—H4A	0.9600
C12—H12A	0.9300	C4—H4B	0.9600
C7—C8	1.385 (8)	C4—H4C	0.9600

O5—Ni1—O1	88.16 (12)	C3—O2—Ni1	123.9 (3)
O5—Ni1—O2	176.74 (14)	C3—O2—K1ⁱ	129.1 (3)
O1—Ni1—O2	92.83 (11)	Ni1—O2—K1ⁱ	88.38 (11)
O5—Ni1—O4	92.61 (12)	C8—O4—Ni1	126.0 (3)
O1—Ni1—O4	174.52 (16)	C8—O4—K1ⁱ	129.3 (2)
O2—Ni1—O4	86.69 (12)	Ni1—O4—K1ⁱ	88.31 (11)
O5—Ni1—O6	87.41 (13)	C11—O5—Ni1	127.1 (3)
O1—Ni1—O6	91.71 (14)	C11—O5—K1	125.8 (2)
O2—Ni1—O6	89.46 (13)	Ni1—O5—K1	90.46 (11)
O4—Ni1—O6	93.75 (13)	C13—C12—C11	123.4 (5)
O5—Ni1—O3	92.28 (12)	C13—C12—H12A	118.3
O1—Ni1—O3	87.63 (12)	C11—C12—H12A	118.3
O2—Ni1—O3	90.86 (13)	C8—C7—C6	125.0 (5)
O4—Ni1—O3	86.92 (13)	C8—C7—H7A	117.5
O6—Ni1—O3	179.28 (13)	C6—C7—H7A	117.5
O5—Ni1—K1	52.40 (8)	O5—C11—C12	127.9 (4)
O1—Ni1—K1	55.17 (8)	O5—C11—C14	115.8 (4)
O2—Ni1—K1	130.50 (9)	C12—C11—C14	116.3 (4)
O4—Ni1—K1	121.53 (8)	O2—C3—C2	125.6 (4)
O6—Ni1—K1	123.87 (10)	O2—C3—C5	115.1 (4)
O3—Ni1—K1	55.47 (8)	C2—C3—C5	119.3 (4)
O5—Ni1—K1ⁱ	122.77 (9)	C13—C15—H15A	109.5
O1—Ni1—K1ⁱ	129.61 (8)	C13—C15—H15B	109.5
O2—Ni1—K1ⁱ	54.42 (8)	H15A—C15—H15B	109.5
O4—Ni1—K1ⁱ	53.97 (8)	C13—C15—H15C	109.5
O6—Ni1—K1ⁱ	55.84 (9)	H15A—C15—H15C	109.5
O3—Ni1—K1ⁱ	124.85 (10)	H15B—C15—H15C	109.5
K1—Ni1—K1ⁱ	174.427 (15)	C8—C10—H10A	109.5
O5—K1—O4ⁱⁱ	157.02 (9)	C8—C10—H10B	109.5
O5—K1—O2ⁱⁱ	95.20 (9)	H10A—C10—H10B	109.5
O4ⁱⁱ—K1—O2ⁱⁱ	61.96 (8)	C8—C10—H10C	109.5
O5—K1—O1	62.77 (9)	H10A—C10—H10C	109.5
O4ⁱⁱ—K1—O1	140.21 (9)	H10B—C10—H10C	109.5
O2ⁱⁱ—K1—O1	157.15 (9)	O1—C1—C2	126.5 (4)
O5—K1—O3	66.63 (9)	O1—C1—C4	114.2 (4)
O4ⁱⁱ—K1—O3	119.10 (13)	C2—C1—C4	119.3 (4)
O2ⁱⁱ—K1—O3	104.63 (11)	O6—C13—C12	125.6 (4)
O1—K1—O3	62.51 (9)	O6—C13—C15	118.8 (4)
O5—K1—O6ⁱⁱ	101.95 (11)	C12—C13—C15	115.6 (5)
O4ⁱⁱ—K1—O6ⁱⁱ	66.85 (9)	C3—C2—C1	128.0 (4)
O2ⁱⁱ—K1—O6ⁱⁱ	63.56 (10)	C3—C2—H2A	116.0
O1—K1—O6ⁱⁱ	124.05 (13)	C1—C2—H2A	116.0
O3—K1—O6ⁱⁱ	163.69 (9)	C6—C9—H9A	109.5
O5—K1—O1W	142.07 (17)	C6—C9—H9B	109.5
O4ⁱⁱ—K1—O1W	55.61 (14)	H9A—C9—H9B	109.5
O2ⁱⁱ—K1—O1W	112.68 (12)	C6—C9—H9C	109.5
O1—K1—O1W	89.75 (13)	H9A—C9—H9C	109.5
O3—K1—O1W	125.28 (15)	H9B—C9—H9C	109.5
O6ⁱⁱ—K1—O1W	70.95 (15)	O3—C6—C7	124.5 (5)
O5—K1—Ni1	37.14 (6)	O3—C6—C9	118.7 (4)
O4ⁱⁱ—K1—Ni1	157.34 (11)	C7—C6—C9	116.8 (5)
O2ⁱⁱ—K1—Ni1	120.89 (7)	C11—C14—H14A	109.5
O1—K1—Ni1	37.19 (6)	C11—C14—H14B	109.5
O3—K1—Ni1	38.89 (7)	H14A—C14—H14B	109.5
O6ⁱⁱ—K1—Ni1	135.69 (9)	C11—C14—H14C	109.5
O1W—K1—Ni1	126.39 (11)	H14A—C14—H14C	109.5
O5—K1—Ni1ⁱⁱ	121.61 (7)	H14B—C14—H14C	109.5
O4ⁱⁱ—K1—Ni1ⁱⁱ	37.72 (6)	O4—C8—C7	128.8 (4)
O2ⁱⁱ—K1—Ni1ⁱⁱ	37.20 (6)	O4—C8—C10	114.9 (5)
O1—K1—Ni1ⁱⁱ	160.71 (10)	C7—C8—C10	116.3 (5)
O3—K1—Ni1ⁱⁱ	136.70 (9)	C3—C5—H5A	109.5
O6ⁱⁱ—K1—Ni1ⁱⁱ	38.56 (7)	C3—C5—H5B	109.5
O1W—K1—Ni1ⁱⁱ	76.61 (11)	H5A—C5—H5B	109.5
Ni1—K1—Ni1ⁱⁱ	156.19 (3)	C3—C5—H5C	109.5
C6—O3—Ni1	128.6 (3)	H5A—C5—H5C	109.5
C6—O3—K1	125.6 (2)	H5B—C5—H5C	109.5
Ni1—O3—K1	85.64 (11)	C1—C4—H4A	109.5
C13—O6—Ni1	128.5 (2)	C1—C4—H4B	109.5
C13—O6—K1ⁱ	128.2 (3)	H4A—C4—H4B	109.5
Ni1—O6—K1ⁱ	85.60 (13)	C1—C4—H4C	109.5
C1—O1—Ni1	122.7 (3)	H4A—C4—H4C	109.5
C1—O1—K1	128.0 (3)	H4B—C4—H4C	109.5
Ni1—O1—K1	87.65 (11)

Symmetry codes: (i) x−1/2, −y+1/2, z; (ii) x+1/2, −y+1/2, z.

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Potassium tris­(acetyl­acetonato)­nickelate(II) 0.3-hydrate

Supporting information

Key indicators

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Potassium tris(acetylacetonato)nickelate(II) 0.3-hydrate