A novel three-dimensional Sr^II coordination poly­mer based on benzene-1,2,4,5-tetra­carboxyl­ate: hydro­thermal synthesis, crystal structure and spectroscopic and thermal studies

Coordination of the anions of benzene­carb­oxy­lic acids with metal cations leads to coordination polymers with various structural features. Very few examples of strontium-based structures have been reported. A new three-dimensional coordination polymer, namely poly[aqua­(μ₁₂-benzene-1,2,4,5-tetra­carboxyl­ato)distrontium(II)], [Sr₂(C₁₀H₂O₈)(H₂O)]_n, has been synthesized under hydro­thermal conditions and characterized by thermal analysis, vibrational spectroscopy (Raman and IR), single-crystal X-ray diffraction and powder X-ray diffraction. The coordination geometries around the two independent Sr^II ions can be described as a distorted dodeca­hedron and a distorted monocapped square anti­prism. The compound features a three-dimensional structure con­­taining inorganic motifs, with two-dimensional layers connected through organic linkers, and possesses a topologic structure of a binodal (6,12) connected alb net with the Schläfli symbol {4¹⁵}₂{4⁴⁸.6¹⁸}. The final product of thermal decomposition is strontium oxide (SrO).

Computing details

Data collection: APEX2 (Bruker, 2011); cell refinement: APEX2 (Bruker, 2011); data reduction: APEX2 (Bruker, 2011); program(s) used to solve structure: SIR2002 (Burla et al., 2005); program(s) used to refine structure: SHELXL (Sheldrick, 2008) within WinGX (Farrugia, 2012); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg & Berndt, 2001); software used to prepare material for publication: WinGX (Farrugia, 2012) and CRYSCAL (T. Roisnel, local program).

Poly[aqua(µ₁₂-benzene-1,2,4,5-tetracarboxylato)distrontium(II)]

Crystal data

[Sr2(C10H2O8)(H2O)]	F(000) = 848
Mr = 443.37	Dx = 2.714 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 2975 reflections
a = 8.1694 (3) Å	θ = 3.6–29.9°
b = 17.2478 (5) Å	µ = 9.88 mm^−1
c = 7.7689 (2) Å	T = 295 K
β = 97.521 (1)°	Cube, colorless
V = 1085.25 (6) Å^3	0.15 × 0.14 × 0.14 mm
Z = 4

Data collection

Bruker APEXII diffractometer	1350 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.025
CCD rotation images, thin slices scans	θmax = 30.0°, θmin = 3.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	h = −11→11
Tmin = 0.570, Tmax = 0.746	k = −23→24
5421 measured reflections	l = −10→7
1576 independent reflections

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)] = 0.021	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.050	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0232P)^2 + 0.9793P] where P = (Fo^2 + 2Fc^2)/3
1576 reflections	(Δ/σ)max < 0.001
101 parameters	Δρmax = 0.51 e Å^−3
0 restraints	Δρmin = −0.41 e Å^−3

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles

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
Sr1	0.00000	0.22191 (1)	−0.25000	0.0125 (1)
Sr2	0.00000	0.17126 (2)	0.25000	0.0177 (1)
O1	0.13337 (18)	0.12155 (9)	−0.0374 (2)	0.0176 (4)
O1W	0.00000	0.01583 (14)	0.25000	0.0256 (8)
O2	0.29995 (18)	0.16737 (9)	0.1860 (2)	0.0172 (4)
O3	0.5143 (2)	0.21210 (8)	−0.0560 (2)	0.0177 (4)
O4	0.7637 (2)	0.16316 (9)	−0.0831 (3)	0.0283 (6)
C1	0.2720 (3)	0.12313 (11)	0.0560 (3)	0.0124 (5)
C2	0.3962 (2)	0.06262 (11)	0.0233 (3)	0.0115 (5)
C3	0.3458 (3)	−0.01361 (11)	0.0457 (3)	0.0132 (5)
C4	0.5528 (2)	0.07662 (11)	−0.0234 (3)	0.0113 (5)
C5	0.6158 (3)	0.15688 (12)	−0.0566 (3)	0.0144 (6)
H1W	0.061 (5)	−0.009 (2)	0.322 (5)	0.049 (11)*
H3	0.24125	−0.02255	0.07657	0.0159*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sr1	0.0141 (1)	0.0104 (1)	0.0130 (1)	0.0000	0.0016 (1)	0.0000
Sr2	0.0199 (2)	0.0114 (1)	0.0246 (2)	0.0000	0.0136 (1)	0.0000
O1	0.0148 (7)	0.0176 (7)	0.0193 (8)	0.0055 (6)	−0.0015 (6)	0.0004 (6)
O1W	0.0271 (13)	0.0181 (12)	0.0310 (14)	0.0000	0.0014 (11)	0.0000
O2	0.0147 (7)	0.0164 (7)	0.0212 (8)	−0.0004 (6)	0.0048 (6)	−0.0069 (6)
O3	0.0238 (8)	0.0105 (7)	0.0192 (8)	0.0035 (6)	0.0039 (6)	0.0009 (6)
O4	0.0216 (9)	0.0179 (8)	0.0495 (12)	−0.0056 (7)	0.0200 (8)	−0.0037 (8)
C1	0.0133 (9)	0.0096 (8)	0.0152 (9)	0.0000 (7)	0.0053 (7)	0.0027 (8)
C2	0.0117 (9)	0.0087 (9)	0.0138 (9)	0.0027 (7)	0.0010 (7)	−0.0009 (7)
C3	0.0105 (9)	0.0119 (9)	0.0177 (10)	0.0004 (7)	0.0036 (7)	−0.0007 (8)
C4	0.0113 (9)	0.0100 (8)	0.0130 (9)	0.0011 (7)	0.0026 (7)	−0.0009 (7)
C5	0.0178 (10)	0.0121 (9)	0.0145 (10)	−0.0009 (8)	0.0062 (8)	−0.0012 (8)

Geometric parameters (Å, º)

Sr1—O1	2.5378 (15)	Sr2—O4^i	3.022 (2)
Sr1—O4^i	2.6627 (18)	Sr2—O4^viii	3.022 (2)
Sr1—O1^ii	2.5378 (15)	O1—C1	1.263 (3)
Sr1—O4^iii	2.6627 (18)	O2—C1	1.263 (3)
Sr1—O2^iv	2.5204 (15)	O3—C5	1.263 (3)
Sr1—O3^iv	2.6520 (15)	O4—C5	1.257 (3)
Sr1—O2^v	2.5204 (15)	O1W—H1W^vi	0.82 (4)
Sr1—O3^v	2.6520 (15)	O1W—H1W	0.82 (4)
Sr2—O1	2.7467 (15)	C1—C2	1.500 (3)
Sr2—O1W	2.681 (2)	C2—C3	1.395 (3)
Sr2—O2	2.5642 (15)	C2—C4	1.396 (2)
Sr2—O1^vi	2.7467 (15)	C3—C4^ix	1.391 (3)
Sr2—O2^vi	2.5642 (15)	C4—C5	1.511 (3)
Sr2—O3^iv	2.5073 (15)	C3—H3	0.9300
Sr2—O3^vii	2.5073 (15)
O1—Sr1—O4^i	72.56 (5)	O1^vi—Sr2—O2^vi	48.96 (5)
O1—Sr1—O1^ii	93.99 (5)	O1^vi—Sr2—O3^iv	138.32 (5)
O1—Sr1—O4^iii	77.32 (6)	O1^vi—Sr2—O3^vii	75.76 (5)
O1—Sr1—O2^iv	100.16 (5)	O1—Sr2—O4^i	64.30 (4)
O1—Sr1—O3^iv	76.99 (5)	O1^vi—Sr2—O4^i	113.88 (4)
O1—Sr1—O2^v	149.01 (5)	O2^vi—Sr2—O3^iv	99.62 (5)
O1—Sr1—O3^v	144.16 (5)	O2^vi—Sr2—O3^vii	82.82 (5)
O1^ii—Sr1—O4^i	77.32 (6)	O2—Sr2—O4^i	110.62 (5)
O4^i—Sr1—O4^iii	135.26 (5)	O2^vi—Sr2—O4^i	69.24 (5)
O2^iv—Sr1—O4^i	133.24 (6)	O3^iv—Sr2—O3^vii	73.28 (5)
O3^iv—Sr1—O4^i	66.86 (6)	O3^iv—Sr2—O3^vii	73.28 (5)
O2^v—Sr1—O4^i	83.78 (5)	O3^iv—Sr2—O4^i	63.14 (5)
O3^v—Sr1—O4^i	136.03 (6)	O3^vii—Sr2—O4^i	121.73 (5)
O1^ii—Sr1—O4^iii	72.56 (5)	O1W—Sr2—O4^i	87.35 (3)
O1^ii—Sr1—O2^iv	149.01 (5)	Sr1—O1—Sr2	97.70 (5)
O1^ii—Sr1—O3^iv	144.16 (5)	Sr1—O1—C1	129.46 (13)
O1^ii—Sr1—O2^v	100.16 (5)	Sr2—O1—C1	86.99 (13)
O1^ii—Sr1—O3^v	76.99 (5)	Sr2—O2—C1	95.37 (14)
O2^iv—Sr1—O4^iii	83.78 (5)	Sr1^iv—O2—Sr2	123.60 (6)
O3^iv—Sr1—O4^iii	136.03 (6)	Sr1^iv—O2—C1	131.33 (14)
O2^v—Sr1—O4^iii	133.24 (6)	Sr1^iv—O3—C5	115.65 (14)
O3^v—Sr1—O4^iii	66.86 (6)	Sr2^iv—O3—C5	125.57 (14)
O2^iv—Sr1—O3^iv	66.52 (5)	Sr1^iv—O3—Sr2^iv	100.98 (5)
O2^iv—Sr1—O2^v	81.48 (5)	Sr1^x—O4—C5	152.44 (16)
O2^iv—Sr1—O3^v	75.41 (5)	H1W—O1W—H1W^vi	117 (4)
O2^v—Sr1—O3^iv	75.41 (5)	Sr2—O1W—H1W^vi	122 (3)
O3^iv—Sr1—O3^v	129.17 (4)	Sr2—O1W—H1W	122 (3)
O2^v—Sr1—O3^v	66.52 (5)	O2—C1—C2	120.0 (2)
O1—Sr2—O1W	71.81 (3)	O1—C1—C2	117.60 (18)
O1—Sr2—O2	48.96 (5)	O1—C1—O2	121.8 (2)
O1—Sr2—O1^vi	143.62 (5)	C1—C2—C3	114.66 (17)
O1—Sr2—O2^vi	129.81 (5)	C1—C2—C4	125.94 (18)
O1—Sr2—O3^iv	75.76 (5)	C3—C2—C4	119.40 (18)
O1—Sr2—O3^vii	138.32 (5)	C2—C3—C4^ix	122.0 (2)
O1W—Sr2—O2	88.50 (4)	C3^ix—C4—C5	118.22 (18)
O1^vi—Sr2—O1W	71.81 (3)	C2—C4—C5	123.18 (17)
O1W—Sr2—O2^vi	88.50 (4)	C2—C4—C3^ix	118.57 (18)
O1W—Sr2—O3^iv	143.36 (3)	O3—C5—O4	125.5 (2)
O1W—Sr2—O3^vii	143.36 (3)	O3—C5—C4	116.9 (2)
O1^vi—Sr2—O2	129.81 (5)	O4—C5—C4	117.60 (18)
O2—Sr2—O2^vi	177.00 (5)	C2—C3—H3	119.00
O2—Sr2—O3^iv	82.82 (5)	C4^ix—C3—H3	119.00
O2—Sr2—O3^vii	99.62 (5)
O4^i—Sr1—O1—Sr2	−48.46 (5)	O3^iv—Sr2—O1—Sr1	−22.44 (5)
O1^ii—Sr1—O1—Sr2	−123.84 (5)	O3^vii—Sr2—O1—Sr1	−65.44 (8)
O4^iii—Sr1—O1—Sr2	165.04 (6)	Sr1—O1—C1—O2	71.4 (3)
O2^iv—Sr1—O1—Sr2	83.85 (5)	Sr2—O1—C1—O2	−26.1 (2)
O3^iv—Sr1—O1—Sr2	21.04 (5)	Sr1—O1—C1—C2	−117.14 (17)
O2^v—Sr1—O1—Sr2	−6.49 (12)	Sr2—O1—C1—C2	145.36 (18)
O3^v—Sr1—O1—Sr2	162.96 (6)	Sr2—O2—C1—O1	28.2 (2)
O4^i—Sr1—O1—C1	−140.91 (19)	Sr1^iv—O2—C1—O1	−117.1 (2)
O1^ii—Sr1—O1—C1	143.72 (18)	Sr2—O2—C1—C2	−143.05 (17)
O4^iii—Sr1—O1—C1	72.60 (18)	Sr1^iv—O2—C1—C2	71.6 (2)
O2^iv—Sr1—O1—C1	−8.60 (19)	Sr1^iv—O3—C5—C4	89.2 (2)
O3^iv—Sr1—O1—C1	−71.41 (18)	Sr1^iv—O3—C5—O4	−91.1 (3)
O2^v—Sr1—O1—C1	−98.93 (19)	Sr2^iv—O3—C5—O4	36.0 (3)
O3^v—Sr1—O1—C1	70.5 (2)	Sr2^iv—O3—C5—C4	−143.71 (16)
O3—Sr1^iv—O2—Sr2	−137.24 (8)	Sr1^x—O4—C5—C4	138.3 (3)
O3—Sr1^iv—O2—C1	−0.03 (18)	Sr1^x—O4—C5—O3	−41.4 (5)
O2—Sr1^iv—O3—C5	−90.66 (15)	O1—C1—C2—C3	−60.3 (3)
O1W—Sr2—O1—Sr1	140.26 (5)	O2—C1—C2—C3	111.3 (2)
O2—Sr2—O1—Sr1	−115.30 (7)	O2—C1—C2—C4	−67.7 (3)
O1^vi—Sr2—O1—Sr1	140.26 (6)	O1—C1—C2—C4	120.7 (2)
O1W—Sr2—O1—C1	−90.31 (11)	C1—C2—C4—C3^ix	178.8 (2)
O2—Sr2—O1—C1	14.14 (11)	C3—C2—C4—C5	177.8 (2)
O1^vi—Sr2—O1—C1	−90.31 (13)	C1—C2—C3—C4^ix	−178.9 (2)
O2^vi—Sr2—O1—C1	−162.27 (11)	C4—C2—C3—C4^ix	0.2 (3)
O3^iv—Sr2—O1—C1	106.99 (12)	C1—C2—C4—C5	−3.2 (4)
O3^vii—Sr2—O1—C1	63.99 (14)	C3—C2—C4—C3^ix	−0.2 (3)
O1—Sr2—O2—C1	−14.18 (11)	C2—C3—C4^ix—C5^ix	177.9 (2)
O1W—Sr2—O2—C1	52.79 (12)	C2—C3—C4^ix—C2^ix	−0.2 (3)
O1^vi—Sr2—O2—C1	117.43 (12)	C3^ix—C4—C5—O4	−8.0 (3)
O3^iv—Sr2—O2—C1	−91.54 (12)	C2—C4—C5—O3	−6.3 (3)
O3^vii—Sr2—O2—C1	−163.15 (12)	C2—C4—C5—O4	174.0 (2)
O1—Sr2—O2—Sr1^iv	135.00 (10)	C3^ix—C4—C5—O3	171.7 (2)
O2^vi—Sr2—O1—Sr1	68.30 (7)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W···O1^xi	0.82 (4)	2.27 (4)	3.010 (2)	151 (4)
C3—H3···O4^ix	0.9300	2.4300	2.758 (3)	101.00

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