Crystal structure of catena-poly[[[di­aqua­bis­(2,4,6-tri­methyl­benzoato-κO)cobalt(II)]-μ-aqua-κ²O:O] dihydrate]

In {[Co(C₁₀H₁₁O₂)₂(H₂O)₃]·2H₂O}_n, the Co^II atom is coordinated by two TMB anions and two water mol­ecules in the basal plane, while another water mol­ecule bridges the Co^II atoms in the apical directions, forming polymeric chains running along [001].

Key indicators

• Single-crystal X-ray study
• T = 296 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.060
• wR factor = 0.166
• Data-to-parameter ratio = 18.4

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT094_ALERT_2_B Ratio of Maximum / Minimum Residual Density ....       4.18 Report
PLAT420_ALERT_2_B D-H Without Acceptor       O5     --  H51    ...     Please Check

Alert level C
DIFMX02_ALERT_1_C  The maximum difference density is > 0.1*ZMAX*0.75
            The relevant atom site should be identified.
PLAT097_ALERT_2_C Large Reported Max.  (Positive) Residual Density       2.18 eA-3
PLAT220_ALERT_2_C Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range        3.1 Ratio
PLAT341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0061 Ang.
PLAT481_ALERT_4_C Long D...A H-Bond Reported C6     ..  CG1     ..       4.06 Ang.
PLAT905_ALERT_3_C Negative K value in the Analysis of Variance ...     -0.363 Report
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          7 Report
PLAT971_ALERT_2_C Check Calcd Residual Density  0.91A From     Co1       2.13 eA-3

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          8 Note
PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          3 Report
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          1 Info
PLAT005_ALERT_5_G No Embedded Refinement Details found  in the CIF     Please Do !
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large       9.97 Why ?
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............         74 Note
PLAT899_ALERT_4_G SHELXL97   is Deprecated and Succeeded by SHELXL       2014 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         13 Note
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          3 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   2 ALERT level B = A potentially serious problem, consider carefully
   8 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   9 ALERT level G = General information/check it is not something unexpected

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   9 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

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Computing details

Data collection: APEX2 (Bruker, 2012); cell refinement: SAINT (Bruker, 2012); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: WinGX publication routines (Farrugia, 2012) and PLATON (Spek, 2009).

catena-Poly[[[diaquabis(2,4,6-trimethylbenzoato-κO)cobalt(II)]-µ-aqua-κ²O:O] dihydrate]

Crystal data

[Co(C10H11O2)2(H2O)3]·2H2O	F(000) = 1004
Mr = 475.39	Dx = 1.304 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 9882 reflections
a = 29.5261 (5) Å	θ = 2.8–28.1°
b = 10.1413 (2) Å	µ = 0.75 mm^−1
c = 8.0906 (2) Å	T = 296 K
β = 91.894 (4)°	Block, translucent light pink
V = 2421.27 (9) Å^3	0.35 × 0.29 × 0.20 mm
Z = 4

Data collection

Bruker SMART BREEZE CCD diffractometer	2957 independent reflections
Radiation source: fine-focus sealed tube	2448 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.058
φ and ω scans	θmax = 28.2°, θmin = 1.4°
Absorption correction: multi-scan SADABS; Bruker, 2012	h = −38→39
Tmin = 0.779, Tmax = 0.864	k = −12→13
25445 measured reflections	l = −10→10

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)] = 0.060	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.166	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	w = 1/[σ^2(Fo^2) + (0.0725P)^2 + 9.9721P] where P = (Fo^2 + 2Fc^2)/3
2957 reflections	(Δ/σ)max < 0.001
161 parameters	Δρmax = 2.18 e Å^−3
74 restraints	Δρmin = −0.52 e Å^−3

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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 (Ų)

	x	y	z	Uiso*/Ueq
Co1	0.5000	0.5000	0.5000	0.02399 (18)
O1	0.55057 (8)	0.6264 (2)	0.4251 (3)	0.0409 (6)
O2	0.57111 (9)	0.7216 (3)	0.6626 (3)	0.0503 (7)
O3	0.45248 (10)	0.6292 (3)	0.4084 (3)	0.0492 (7)
H31	0.4484 (17)	0.625 (6)	0.310 (2)	0.086 (17)*
H32	0.4289 (10)	0.656 (4)	0.446 (5)	0.057 (13)*
O4	0.5000	0.4132 (3)	0.2500	0.0274 (6)
H41	0.5249 (8)	0.378 (4)	0.237 (5)	0.048 (10)*
O5	0.37711 (14)	0.7250 (4)	0.5521 (4)	0.0768 (10)
H51	0.3607 (18)	0.785 (4)	0.522 (7)	0.103 (15)*
H52	0.385 (2)	0.740 (6)	0.649 (3)	0.100 (15)*
C1	0.57564 (11)	0.7012 (3)	0.5121 (4)	0.0348 (6)
C2	0.61375 (11)	0.7694 (3)	0.4254 (4)	0.0366 (7)
C3	0.65665 (13)	0.7129 (4)	0.4284 (5)	0.0509 (9)
C4	0.69080 (15)	0.7756 (5)	0.3429 (6)	0.0625 (11)
H4	0.7196	0.7386	0.3439	0.075*
C5	0.68271 (16)	0.8917 (5)	0.2564 (5)	0.0647 (12)
C6	0.64030 (15)	0.9461 (4)	0.2567 (5)	0.0567 (11)
H6	0.6349	1.0245	0.1997	0.068*
C7	0.60467 (13)	0.8874 (4)	0.3403 (4)	0.0450 (8)
C8	0.55866 (16)	0.9483 (5)	0.3372 (7)	0.0689 (12)
H8A	0.5409	0.9133	0.2458	0.103*
H8B	0.5614	1.0421	0.3252	0.103*
H8C	0.5441	0.9286	0.4387	0.103*
C9	0.7209 (2)	0.9563 (8)	0.1634 (8)	0.109 (2)
H9A	0.7152	0.9467	0.0465	0.164*
H9B	0.7491	0.9145	0.1941	0.164*
H9C	0.7225	1.0482	0.1911	0.164*
C10	0.66644 (18)	0.5874 (5)	0.5233 (7)	0.0777 (15)
H10A	0.6629	0.6028	0.6391	0.117*
H10B	0.6970	0.5597	0.5049	0.117*
H10C	0.6457	0.5198	0.4860	0.117*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0380 (3)	0.0218 (3)	0.0124 (3)	−0.00099 (18)	0.00338 (18)	−0.00010 (16)
O1	0.0549 (14)	0.0470 (13)	0.0210 (9)	−0.0202 (10)	0.0055 (9)	−0.0019 (9)
O2	0.0670 (16)	0.0616 (16)	0.0227 (10)	−0.0243 (13)	0.0073 (10)	−0.0082 (10)
O3	0.0633 (16)	0.0626 (17)	0.0221 (11)	0.0257 (13)	0.0050 (10)	0.0023 (11)
O4	0.0375 (15)	0.0275 (13)	0.0175 (12)	0.000	0.0044 (10)	0.000
O5	0.087 (2)	0.094 (3)	0.0492 (18)	0.032 (2)	−0.0007 (16)	−0.0010 (18)
C1	0.0459 (16)	0.0352 (15)	0.0234 (13)	−0.0057 (12)	0.0017 (11)	0.0016 (11)
C2	0.0439 (16)	0.0405 (16)	0.0255 (13)	−0.0142 (13)	0.0024 (11)	−0.0034 (12)
C3	0.051 (2)	0.056 (2)	0.046 (2)	−0.0079 (17)	0.0059 (15)	0.0018 (17)
C4	0.048 (2)	0.084 (3)	0.056 (2)	−0.011 (2)	0.0104 (17)	0.005 (2)
C5	0.063 (3)	0.088 (3)	0.043 (2)	−0.033 (2)	0.0041 (18)	0.011 (2)
C6	0.072 (3)	0.057 (2)	0.0398 (19)	−0.027 (2)	−0.0063 (17)	0.0137 (17)
C7	0.055 (2)	0.0468 (19)	0.0326 (16)	−0.0138 (15)	−0.0030 (14)	0.0054 (14)
C8	0.071 (3)	0.060 (3)	0.075 (3)	0.002 (2)	−0.005 (2)	0.024 (2)
C9	0.081 (4)	0.163 (6)	0.083 (4)	−0.057 (4)	0.011 (3)	0.042 (4)
C10	0.070 (3)	0.068 (3)	0.095 (4)	0.015 (2)	0.015 (3)	0.025 (3)

Geometric parameters (Å, º)

Co1—O1	2.074 (2)	C3—C10	1.509 (6)
Co1—O1^i	2.074 (2)	C4—C5	1.387 (7)
Co1—O3	2.041 (2)	C4—H4	0.9300
Co1—O3^i	2.041 (2)	C5—C9	1.524 (6)
Co1—O4	2.2060 (11)	C6—C5	1.368 (7)
Co1—O4^i	2.2060 (11)	C6—H6	0.9300
O1—C1	1.259 (4)	C7—C6	1.402 (5)
O2—C1	1.246 (4)	C7—C8	1.492 (6)
O3—H31	0.806 (19)	C8—H8A	0.9600
O3—H32	0.818 (18)	C8—H8B	0.9600
O4—Co1^ii	2.2060 (11)	C8—H8C	0.9600
O4—H41	0.827 (18)	C9—H9A	0.9600
O5—H51	0.812 (10)	C9—H9B	0.9600
O5—H52	0.820 (10)	C9—H9C	0.9600
C2—C1	1.513 (4)	C10—H10A	0.9600
C2—C3	1.390 (5)	C10—H10B	0.9600
C2—C7	1.401 (5)	C10—H10C	0.9600
C3—C4	1.395 (5)
O1—Co1—O1^i	180.00 (9)	C4—C3—C10	120.5 (4)
O1—Co1—O4	87.53 (7)	C3—C4—H4	119.3
O1^i—Co1—O4	92.47 (7)	C5—C4—C3	121.5 (4)
O1—Co1—O4^i	92.47 (7)	C5—C4—H4	119.3
O1^i—Co1—O4^i	87.53 (7)	C4—C5—C9	119.7 (5)
O3—Co1—O1	89.44 (11)	C6—C5—C4	118.9 (4)
O3^i—Co1—O1	90.56 (11)	C6—C5—C9	121.4 (5)
O3—Co1—O1^i	90.56 (11)	C5—C6—C7	122.1 (4)
O3^i—Co1—O1^i	89.44 (11)	C5—C6—H6	119.0
O3^i—Co1—O3	180.00 (12)	C7—C6—H6	119.0
O3—Co1—O4	86.80 (8)	C2—C7—C6	117.7 (4)
O3^i—Co1—O4	93.20 (8)	C2—C7—C8	121.4 (3)
O3—Co1—O4^i	93.20 (8)	C6—C7—C8	120.9 (4)
O3^i—Co1—O4^i	86.80 (8)	C7—C8—H8A	109.5
O4^i—Co1—O4	180.0	C7—C8—H8B	109.5
C1—O1—Co1	128.67 (19)	C7—C8—H8C	109.5
Co1—O3—H32	131 (3)	H8A—C8—H8B	109.5
Co1—O3—H31	114 (4)	H8A—C8—H8C	109.5
H32—O3—H31	107 (4)	H8B—C8—H8C	109.5
Co1—O4—Co1^ii	132.95 (13)	C5—C9—H9A	109.5
Co1—O4—H41	108 (3)	C5—C9—H9B	109.5
Co1^ii—O4—H41	92 (3)	C5—C9—H9C	109.5
H51—O5—H52	107 (4)	H9A—C9—H9B	109.5
O1—C1—C2	116.7 (3)	H9A—C9—H9C	109.5
O2—C1—O1	124.5 (3)	H9B—C9—H9C	109.5
O2—C1—C2	118.9 (3)	C3—C10—H10A	109.5
C3—C2—C1	119.7 (3)	C3—C10—H10B	109.5
C3—C2—C7	121.3 (3)	C3—C10—H10C	109.5
C7—C2—C1	119.0 (3)	H10A—C10—H10B	109.5
C2—C3—C4	118.5 (4)	H10A—C10—H10C	109.5
C2—C3—C10	121.1 (4)	H10B—C10—H10C	109.5
O3—Co1—O1—C1	105.4 (3)	C1—C2—C3—C10	−2.7 (6)
O3^i—Co1—O1—C1	−74.6 (3)	C7—C2—C3—C4	−0.7 (6)
O4—Co1—O1—C1	−167.8 (3)	C7—C2—C3—C10	178.7 (4)
O4^i—Co1—O1—C1	12.2 (3)	C1—C2—C7—C6	−178.0 (3)
O1—Co1—O4—Co1^ii	−46.09 (7)	C1—C2—C7—C8	1.5 (5)
O1^i—Co1—O4—Co1^ii	133.91 (7)	C3—C2—C7—C6	0.6 (5)
O3—Co1—O4—Co1^ii	43.49 (9)	C3—C2—C7—C8	−179.9 (4)
O3^i—Co1—O4—Co1^ii	−136.51 (9)	C2—C3—C4—C5	0.1 (7)
Co1—O1—C1—O2	−7.3 (5)	C10—C3—C4—C5	−179.3 (5)
Co1—O1—C1—C2	172.4 (2)	C3—C4—C5—C6	0.6 (7)
C3—C2—C1—O1	−94.3 (4)	C3—C4—C5—C9	−179.5 (5)
C3—C2—C1—O2	85.4 (4)	C7—C6—C5—C4	−0.7 (7)
C7—C2—C1—O1	84.4 (4)	C7—C6—C5—C9	179.4 (5)
C7—C2—C1—O2	−95.9 (4)	C2—C7—C6—C5	0.1 (6)
C1—C2—C3—C4	177.9 (3)	C8—C7—C6—C5	−179.4 (4)

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

Hydrogen-bond geometry (Å, º)

Cg1 is the centroid of the C2–C7 ring.

D—H···A	D—H	H···A	D···A	D—H···A
O3—H31···O1^ii	0.80 (2)	1.90 (2)	2.697 (3)	170 (5)
O3—H32···O5	0.82 (3)	1.91 (3)	2.724 (5)	174 (3)
O4—H41···O2^iii	0.83 (3)	1.82 (3)	2.622 (3)	164 (4)
O5—H52···O2^iv	0.82 (3)	1.98 (4)	2.726 (4)	151 (6)
C10—H10C···O5^i	0.96	2.59	3.466 (7)	152
C6—H6···Cg1^v	0.93	3.28	4.063 (4)	143
C9—H9A···Cg1^v	0.96	3.40	3.961 (7)	120

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, y, −z+1/2; (iii) x, −y+1, z−1/2; (iv) −x+1, y, −z+3/2; (v) −x+1/2, y+3/2, −z−1/2.