Tetra­aqua­bis(4-formyl­benzoato-κO)nickel(II) tetra­hydrate

In the title compound, [Ni(C₈H₅O₃)₂(H₂O)₄]·4H₂O the Ni atom (site symmetry ) 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.

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

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Computing details

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)

Crystal data

[Ni(C8H5O3)2(H2O)4]·4H2O	Z = 1
Mr = 501.08	F(000) = 262
Triclinic, P1	Dx = 1.563 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.124 (4) Å	Cell parameters from 4974 reflections
b = 7.470 (4) Å	θ = 3.1–27.5°
c = 11.488 (8) Å	µ = 0.98 mm^−1
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) Å^3

Data collection

Rigaku RAXIS-RAPID IP diffractometer	2424 independent reflections
Radiation source: fine-focus sealed tube	2226 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.016
ω scan	θmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan ABSCOR (Higashi, 1995)	h = −9→8
Tmin = 0.695, Tmax = 0.835	k = −9→9
5303 measured reflections	l = −14→14

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.028	Hydrogen site location: difmap and geom
wR(F^2) = 0.080	H atoms treated by a mixture of independent and constrained refinement
S = 1.10	w = 1/[σ^2(Fo^2) + (0.0537P)^2 + 0.0268P] where P = (Fo^2 + 2Fc^2)/3
2424 reflections	(Δ/σ)max = 0.001
174 parameters	Δρmax = 0.34 e Å^−3
12 restraints	Δρmin = −0.20 e Å^−3

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

	x	y	z	Uiso*/Ueq
Ni1	0.5000	0.5000	0.5000	0.02825 (11)
O1	0.45641 (18)	0.39413 (19)	0.36228 (10)	0.0359 (3)
O2	0.76977 (19)	0.3173 (2)	0.25347 (12)	0.0485 (3)
O3	0.0882 (2)	0.2381 (2)	−0.11446 (13)	0.0518 (4)
O1W	0.79956 (18)	0.47677 (19)	0.42522 (12)	0.0384 (3)
O2W	0.6223 (2)	0.21284 (19)	0.59934 (12)	0.0409 (3)
O3W	1.2053 (3)	0.1536 (3)	0.49239 (16)	0.0606 (4)
O4W	1.0246 (2)	−0.1029 (2)	0.28328 (14)	0.0564 (4)
C1	0.5820 (2)	0.3395 (2)	0.26978 (14)	0.0301 (3)
C2	0.4993 (2)	0.3033 (2)	0.17055 (13)	0.0281 (3)
C3	0.2926 (3)	0.3236 (3)	0.18304 (14)	0.0345 (3)
H3	0.2068	0.3532	0.2547	0.041*
C4	0.2147 (3)	0.3000 (3)	0.08915 (15)	0.0359 (3)
H4	0.0770	0.3129	0.0978	0.043*
C5	0.3425 (3)	0.2569 (2)	−0.01813 (14)	0.0319 (3)
C6	0.5488 (3)	0.2357 (2)	−0.03069 (14)	0.0338 (3)
H6	0.6343	0.2066	−0.1025	0.041*
C7	0.6273 (3)	0.2580 (2)	0.06358 (15)	0.0333 (3)
H7	0.7658	0.2426	0.0553	0.040*
C8	0.2624 (3)	0.2311 (3)	−0.11929 (15)	0.0394 (4)
H8	0.3507	0.2082	−0.1908	0.047*
H11	0.812 (4)	0.428 (3)	0.3619 (13)	0.057 (7)*
H12	0.893 (4)	0.391 (3)	0.4686 (19)	0.085 (9)*
H21	0.720 (3)	0.190 (4)	0.6403 (19)	0.072 (8)*
H22	0.661 (4)	0.119 (3)	0.559 (2)	0.085 (9)*
H31	1.328 (3)	0.145 (6)	0.482 (2)	0.119 (14)*
H32	1.159 (3)	0.147 (4)	0.5663 (11)	0.065 (8)*
H41	0.967 (5)	0.0243 (14)	0.269 (3)	0.105 (12)*
H42	1.001 (4)	−0.151 (3)	0.2307 (17)	0.060 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.02467 (15)	0.03378 (16)	0.02892 (16)	−0.01129 (11)	−0.00468 (10)	−0.01011 (11)
O1	0.0305 (6)	0.0498 (7)	0.0325 (6)	−0.0172 (5)	−0.0015 (4)	−0.0167 (5)
O2	0.0306 (6)	0.0758 (9)	0.0476 (7)	−0.0226 (6)	0.0011 (5)	−0.0297 (7)
O3	0.0492 (8)	0.0590 (8)	0.0545 (8)	−0.0189 (7)	−0.0171 (6)	−0.0202 (7)
O1W	0.0305 (6)	0.0468 (7)	0.0420 (7)	−0.0161 (5)	−0.0038 (5)	−0.0146 (6)
O2W	0.0419 (7)	0.0381 (6)	0.0424 (7)	−0.0125 (5)	−0.0132 (5)	−0.0066 (5)
O3W	0.0732 (11)	0.0589 (9)	0.0624 (10)	−0.0370 (9)	−0.0151 (8)	−0.0070 (8)
O4W	0.0533 (8)	0.0593 (9)	0.0596 (9)	−0.0126 (7)	−0.0225 (7)	−0.0236 (8)
C1	0.0285 (7)	0.0306 (7)	0.0311 (7)	−0.0104 (6)	−0.0049 (6)	−0.0070 (6)
C2	0.0292 (7)	0.0271 (7)	0.0283 (7)	−0.0111 (6)	−0.0041 (6)	−0.0053 (5)
C3	0.0321 (8)	0.0450 (9)	0.0285 (7)	−0.0170 (7)	0.0009 (6)	−0.0113 (7)
C4	0.0313 (8)	0.0464 (9)	0.0348 (8)	−0.0185 (7)	−0.0027 (6)	−0.0113 (7)
C5	0.0372 (8)	0.0294 (7)	0.0308 (8)	−0.0132 (6)	−0.0058 (6)	−0.0072 (6)
C6	0.0369 (8)	0.0356 (8)	0.0284 (7)	−0.0146 (7)	0.0027 (6)	−0.0104 (6)
C7	0.0304 (8)	0.0366 (8)	0.0342 (8)	−0.0144 (7)	−0.0010 (6)	−0.0094 (6)
C8	0.0478 (10)	0.0373 (8)	0.0339 (8)	−0.0145 (8)	−0.0080 (7)	−0.0103 (7)

Geometric parameters (Å, º)

Ni1—O1	2.048 (2)	O4W—H41	0.845 (10)
Ni1—O1^i	2.048 (2)	O4W—H42	0.844 (9)
Ni1—O2w^i	2.080 (2)	C1—C2	1.504 (2)
Ni1—O1w	2.083 (2)	C2—C7	1.389 (2)
Ni1—O2w	2.080 (2)	C2—C3	1.394 (2)
Ni1—O1w^i	2.083 (2)	C3—C4	1.382 (2)
C1—O1	1.263 (2)	C3—H3	0.9300
C1—O2	1.254 (2)	C4—C5	1.389 (2)
O3—C8	1.210 (2)	C4—H4	0.9300
O1W—H11	0.859 (9)	C5—C6	1.389 (2)
O1W—H12	0.845 (9)	C5—C8	1.473 (2)
O2W—H21	0.855 (9)	C6—C7	1.383 (2)
O2W—H22	0.841 (9)	C6—H6	0.9300
O3W—H31	0.836 (10)	C7—H7	0.9300
O3W—H32	0.847 (9)	C8—H8	0.9300
O1—Ni1—O1^i	180.0	C7—C2—C3	119.75 (14)
O1—Ni1—O1w	93.81 (6)	C7—C2—C1	119.64 (14)
O1—Ni1—O1w^i	86.19 (6)	C3—C2—C1	120.55 (14)
O1—Ni1—O2w	92.37 (7)	C4—C3—C2	120.17 (15)
O1—Ni1—O2w^i	87.63 (7)	C4—C3—H3	119.9
O1w—Ni1—O1w^i	180.0	C2—C3—H3	119.9
O1w—Ni1—O2w	91.58 (6)	C3—C4—C5	119.88 (15)
O1w^i—Ni1—O2w	88.42 (6)	C3—C4—H4	120.1
O2w—Ni1—O2w^i	180.0	C5—C4—H4	120.1
C1—O1—Ni1	127.92 (10)	C4—C5—C6	120.07 (14)
Ni1—O1W—H11	99.7 (16)	C4—C5—C8	120.71 (15)
Ni1—O1W—H12	112 (2)	C6—C5—C8	119.22 (15)
H11—O1W—H12	108.2 (14)	C7—C6—C5	120.05 (15)
Ni1—O2W—H21	115.2 (17)	C7—C6—H6	120.0
Ni1—O2W—H22	113.8 (19)	C5—C6—H6	120.0
H21—O2W—H22	109.5 (15)	C6—C7—C2	120.06 (15)
H31—O3W—H32	111.2 (16)	C6—C7—H7	120.0
H41—O4W—H42	109.4 (15)	C2—C7—H7	120.0
O2—C1—O1	124.73 (14)	O3—C8—C5	123.66 (17)
O2—C1—C2	117.50 (14)	O3—C8—H8	118.2
O1—C1—C2	117.75 (14)	C5—C8—H8	118.2
O2W^i—Ni1—O1—C1	88.22 (14)	C1—C2—C3—C4	176.74 (15)
O2W—Ni1—O1—C1	−91.78 (14)	C2—C3—C4—C5	−0.4 (3)
O1W^i—Ni1—O1—C1	179.96 (14)	C3—C4—C5—C6	0.6 (2)
O1W—Ni1—O1—C1	−0.04 (14)	C3—C4—C5—C8	180.00 (15)
Ni1—O1—C1—O2	9.4 (2)	C4—C5—C6—C7	−0.1 (2)
Ni1—O1—C1—C2	−169.04 (10)	C8—C5—C6—C7	−179.54 (14)
O2—C1—C2—C7	−3.5 (2)	C5—C6—C7—C2	−0.6 (2)
O1—C1—C2—C7	175.14 (14)	C3—C2—C7—C6	0.8 (2)
O2—C1—C2—C3	179.45 (16)	C1—C2—C7—C6	−176.29 (14)
O1—C1—C2—C3	−2.0 (2)	C4—C5—C8—O3	−2.7 (3)
C7—C2—C3—C4	−0.4 (2)	C6—C5—C8—O3	176.65 (17)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H11···O2	0.86 (1)	1.77 (1)	2.607 (2)	163 (2)
O1w—H12···O3w	0.85 (1)	2.18 (2)	2.953 (3)	152 (2)
O2w—H22···O3w^ii	0.84 (1)	2.01 (1)	2.819 (3)	162 (3)
O2w—H21···O4w^ii	0.86 (1)	1.96 (1)	2.803 (2)	170 (2)
O3w—H31···O1^iii	0.84 (1)	2.45 (3)	3.037 (2)	128 (3)
O3w—H32···O4w^ii	0.85 (1)	2.01 (1)	2.812 (3)	158 (2)
O4w—H41···O2	0.85 (1)	2.01 (1)	2.836 (3)	167 (3)
O4w—H42···O3^iv	0.84 (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.