Poly[[μ-aqua-tetraaquabis(μ-2-hydroxy-4-oxocyclobut-1-ene-1,3-diolato)strontium] hemihydrate]

Bouhali, A.; Trifa, C.; Bouacida, S.; Boudaren, C.; Bataille, T.

doi:10.1107/S1600536811028704

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 8| August 2011| Pages m1130-m1131

doi:10.1107/S1600536811028704

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Poly[[μ-aqua-tetraaquabis(μ-2-hydroxy-4-oxocyclobut-1-ene-1,3-diolato)strontium] hemihydrate]

Amira Bouhali,^a Chahrazed Trifa,^a Sofiane Bouacida,^a ^* Chaouki Boudaren ^a and Thierry Bataille ^b

^aUnité de Recherche de Chimie de l'Environnement et Moléculaire Structurale, CHEMS, Université Mentouri–Constantine, 25000 Algeria, and ^bSciences Chimiques de Rennes, UMR 6226 CNRS - Université de Rennes 1, Avenue du Général Leclerc, 35042 Rennes cedex, France
^*Correspondence e-mail: Bouacida_Sofiane@yahoo.fr

(Received 30 June 2011; accepted 17 July 2011; online 23 July 2011)

In the title coordination polymer, {[Sr(C₄HO₄)₂(H₂O)₅]·0.5H₂O}_n, the Sr²⁺ ion is coordinated by three monodentate hydrogensquarate (hsq) anions and six aqua ligands in a distorted SrO₉ monocapped square-antiprismatic geometry. The hsq anions and water molecules bridge the metal ions into infinite sheets lying parallel to (100). The O atom of the uncoordinated water molecule lies on a crystallographic twofold axis. The packing is stabilized by numerous O—H⋯O hydrogen bonds.

Related literature

For the isostructural mixed-metal Ba/Sr analogue of the title compound and background references, see: Trifa et al. (2011 ).

Experimental

Crystal data

[Sr(C₄HO₄)₂(H₂O)₅]·0.5H₂O
M_r = 412.81
Monoclinic, C 2/c
a = 24.885 (3) Å
b = 8.8026 (9) Å
c = 13.8918 (17) Å
β = 119.609 (4)°
V = 2645.7 (5) Å³
Z = 8
Mo Kα radiation
μ = 4.15 mm⁻¹
T = 150 K
0.57 × 0.27 × 0.10 mm

Data collection

Bruker APEXII diffractometer
Absorption correction: multi-scan SADABS (Bruker, 2006 ) T_min = 0.365, T_max = 0.660
9165 measured reflections
3006 independent reflections
2243 reflections with I > 2σ(I)
R_int = 0.037

Refinement

R[F² > 2σ(F²)] = 0.028
wR(F²) = 0.068
S = 1.03
3006 reflections
239 parameters
2 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.42 e Å⁻³
Δρ_min = −0.51 e Å⁻³

Table 1
Selected bond lengths (Å)

Sr1—O1	2.691 (2)
Sr1—O2	2.642 (2)
Sr1—O3	2.690 (2)
Sr1—O4	2.641 (3)
Sr1—O5	2.572 (2)
Sr1—O6	2.6179 (18)
Sr1—O12	2.6646 (16)
Sr1—O14ⁱ	2.5906 (16)
Sr1—O3ⁱⁱ	2.7154 (19)
Symmetry codes: (i) x, y+1, z; (ii) -x+2, -y+2, -z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1A⋯O9ⁱⁱⁱ	0.76 (4)	2.27 (4)	2.983 (3)	158 (4)
O1—H1B⋯O7^iv	0.79 (4)	1.99 (4)	2.715 (2)	153 (4)
O1W—H1W⋯O13ⁱⁱ	0.76 (2)	2.39 (2)	2.801 (2)	115 (2)
O1W—H1W⋯O8^v	0.76 (2)	2.51 (3)	3.118 (2)	138 (3)
O2—H2A⋯O14^vi	0.92 (4)	1.91 (4)	2.794 (3)	161 (4)
O2—H2B⋯O1W^vii	0.70 (4)	2.52 (4)	3.165 (3)	154 (4)
O3—H3A⋯O13ⁱⁱ	0.93 (4)	1.79 (4)	2.712 (3)	174 (3)
O3—H3B⋯O4^viii	0.76 (4)	2.59 (4)	3.172 (3)	136 (3)
O4—H4A⋯O7^ix	0.78 (4)	2.01 (4)	2.785 (3)	177 (4)
O4—H4B⋯O1W	0.87 (4)	2.03 (4)	2.871 (3)	163 (3)
O5—H5A⋯O1^x	0.72 (4)	2.09 (4)	2.787 (3)	166 (4)
O5—H5B⋯O8^xi	0.90 (4)	1.82 (4)	2.716 (3)	175 (4)
O9—H9⋯O12	0.82	1.74	2.548 (3)	169
O11—H11⋯O6^vii	0.82	1.77	2.580 (2)	172
Symmetry codes: (ii) -x+2, -y+2, -z+1; (iii) $[-x+{\script{3\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iv) $[-x+{\script{3\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (v) $[x+{\script{1\over 2}}, -y+{\script{5\over 2}}, z+{\script{1\over 2}}]$ ; (vi) -x+2, -y+1, -z+1; (vii) x, y-1, z; (viii) $[-x+2, y, -z+{\script{1\over 2}}]$ ; (ix) $[-x+{\script{3\over 2}}, -y+{\script{5\over 2}}, -z]$ ; (x) $[x, -y+2, z-{\script{1\over 2}}]$ ; (xi) $[-x+{\script{3\over 2}}, -y+{\script{3\over 2}}, -z]$ .

Data collection: APEX2 (Bruker, 2006); cell refinement: SAINT (Bruker, 2006); data reduction: SAINT; program(s) used to solve structure: SIR2002 (Burla et al., 2003 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ); molecular graphics: ORTEP-3 (Farrugia, 1997 ) and DIAMOND (Brandenburg & Berndt, 2001 ); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811028704/hb5939sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811028704/hb5939Isup2.hkl

checkCIF report

Comment top

As part of our ongoing sturctural studies of alkaline-earth squarate coordination networks (Trifa et al., 2011), we now descibe the synthesis and structure of the title compound, (I).

The asymmetric unit of (I) contains one strontium cation, two hydrogensquarate anions, five aqua ligands and a water molecule (Fig. 1): the O-atom of the latter lies on a crystallographic 2-fold axis.

The strontium atom is coordinated by the O atoms from three hydrogensquarate anions and six water molecules. The ninefold coordination polyhedral of Sr can be described as a monocapped square antiprism SrO₃(H₂O)₆ (Fig. 2).

The hydrogensquarate (HSQ) anions bridge two strontium atoms to form a [Sr2 (H2O)12(HSQ)4] dimer (Fig. 3), thus leading a ribbon of formula [Sr (H2O)6(HC4O4)2] running along [101]. The SrO₉ polyhedra are linked together by sharing two water molecules in the direction of the b axis to build up layers, in between which are located the free water molecules (Fig. 4). The three-dimensionality is ensured by a network of O—H···O hydrogen bonds (Table 2).

Related literature top

For the isostructural mixed-metal Ba/Sr analogue of the title compound and background references, see: Trifa et al. (2011).

Experimental top

Board colourless single crystals of the title compound were obtained by a hydrothermal reaction of an equimolar ratio (1 mmol) of strontium chloride, squaric acid and and 6 ml of water in a 23 ml Teflon-lined acid digestion bomb (Parr) heated for 3 days at 393 K under autogeneous pressure and then cooled down to room temperature. The product obtained were collected by filtration, thoroughly washed with distilled water and ethanol, and finally dried at room temperature.

Computing details top

Data collection: APEXII (Bruker, 2006); cell refinement: SAINT (Bruker, 2006); data reduction: SAINT (Bruker, 2006); program(s) used to solve structure: SIR2002 (Burla et al., 2003); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg & Berndt, 2001); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).

Figures top

	Fig. 1. Drawing of asymetric unit of (I), with displacement ellipsoids drawn at the 50% probability level.
	Fig. 2. The monocapped square antiprism geometry of the Sr atom [Symmetry code: [(i):2 - x, 2 - y, 1 - z, (ii): x, 1 + y, z.].
	Fig. 3. Coordination between squarates ligands and polyhedron unit
	Fig. 4. The crystal structure of the title compound viewed along the b axis, showing the layers.

Poly[[µ-aqua-tetraaquabis(µ-2-hydroxy-4-oxocyclobut-1-ene- 1,3-diolato)strontium] hemihydrate] top

Crystal data top

[Sr(C₄HO₄)₂(H₂O)₅]·0.5H₂O	F(000) = 1656
M_r = 412.81	D_x = 2.073 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 3634 reflections
a = 24.885 (3) Å	θ = 2.5–27.5°
b = 8.8026 (9) Å	µ = 4.15 mm⁻¹
c = 13.8918 (17) Å	T = 150 K
β = 119.609 (4)°	Slab, colourless
V = 2645.7 (5) Å³	0.57 × 0.27 × 0.10 mm
Z = 8

Data collection top

Bruker APEXII diffractometer	2243 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.037
CCD rotation images, thin slices scans	θ_max = 27.5°, θ_min = 2.7°
Absorption correction: multi-scan SADABS (Bruker, 2006)	h = −32→32
T_min = 0.365, T_max = 0.660	k = −8→11
9165 measured reflections	l = −17→18
3006 independent reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.028	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.068	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ²(F_o²) + (0.0273P)² + 1.5645P] where P = (F_o² + 2F_c²)/3
3006 reflections	(Δ/σ)_max = 0.001
239 parameters	Δρ_max = 0.42 e Å⁻³
2 restraints	Δρ_min = −0.51 e Å⁻³

Crystal data top

[Sr(C₄HO₄)₂(H₂O)₅]·0.5H₂O	V = 2645.7 (5) Å³
M_r = 412.81	Z = 8
Monoclinic, C2/c	Mo Kα radiation
a = 24.885 (3) Å	µ = 4.15 mm⁻¹
b = 8.8026 (9) Å	T = 150 K
c = 13.8918 (17) Å	0.57 × 0.27 × 0.10 mm
β = 119.609 (4)°

Data collection top

Bruker APEXII diffractometer	3006 independent reflections
Absorption correction: multi-scan SADABS (Bruker, 2006)	2243 reflections with I > 2σ(I)
T_min = 0.365, T_max = 0.660	R_int = 0.037
9165 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.028	2 restraints
wR(F²) = 0.068	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	Δρ_max = 0.42 e Å⁻³
3006 reflections	Δρ_min = −0.51 e Å⁻³
239 parameters

Special details top

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 e.s.d.'s 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 > 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
Sr1	0.911042 (8)	0.99774 (2)	0.338611 (16)	0.00988 (8)
O1	0.83711 (7)	1.00426 (19)	0.42892 (15)	0.0142 (3)
O2	0.98788 (9)	0.7809 (2)	0.35213 (18)	0.0294 (5)
O3	1.02876 (8)	1.0958 (2)	0.44716 (15)	0.0192 (4)
O4	0.92432 (9)	1.2071 (3)	0.21578 (19)	0.0426 (7)
O5	0.88485 (10)	0.8965 (3)	0.14660 (16)	0.0272 (5)
O6	0.80135 (7)	1.10726 (17)	0.20264 (13)	0.0145 (4)
O7	0.68196 (8)	1.24431 (17)	−0.01295 (14)	0.0167 (4)
O8	0.63364 (7)	0.90554 (19)	−0.10260 (15)	0.0236 (4)
O9	0.74969 (7)	0.76209 (17)	0.11403 (15)	0.0170 (4)
H9	0.7835	0.763	0.1706	0.025*
O11	0.80095 (7)	0.40021 (18)	0.20800 (14)	0.0166 (4)
H11	0.8005	0.3073	0.2116	0.025*
O12	0.84872 (7)	0.73793 (16)	0.29979 (14)	0.0144 (4)
O13	0.95937 (8)	0.5984 (2)	0.52759 (16)	0.0318 (5)
O14	0.91536 (7)	0.25641 (17)	0.43112 (15)	0.0207 (4)
C6	0.75625 (10)	1.0501 (3)	0.1175 (2)	0.0114 (5)
C7	0.70216 (10)	1.1153 (3)	0.0187 (2)	0.0130 (5)
C8	0.67972 (11)	0.9580 (3)	−0.0218 (2)	0.0159 (5)
C9	0.73365 (10)	0.9012 (3)	0.0776 (2)	0.0126 (5)
C11	0.84871 (10)	0.4537 (3)	0.2975 (2)	0.0135 (5)
C12	0.86769 (10)	0.6055 (3)	0.3350 (2)	0.0130 (5)
C13	0.91914 (11)	0.5446 (3)	0.4401 (2)	0.0206 (6)
C14	0.89846 (10)	0.3877 (3)	0.3960 (2)	0.0165 (5)
O1W	1	1.4700 (3)	0.25	0.0446 (9)
H1B	0.8227 (16)	0.926 (4)	0.432 (3)	0.05*
H1A	0.8113 (17)	1.062 (4)	0.401 (3)	0.05*
H5B	0.8812 (15)	0.796 (4)	0.134 (3)	0.05*
H2A	1.0251 (15)	0.776 (4)	0.417 (3)	0.05*
H5A	0.8711 (17)	0.934 (5)	0.094 (3)	0.05*
H3B	1.0439 (16)	1.072 (4)	0.414 (3)	0.05*
H3A	1.0298 (15)	1.201 (4)	0.453 (3)	0.05*
H2B	0.9798 (16)	0.719 (4)	0.316 (3)	0.05*
H4A	0.8953 (17)	1.219 (4)	0.158 (3)	0.05*
H4B	0.9498 (16)	1.284 (4)	0.241 (3)	0.05*
H1W	1.0225 (13)	1.513 (3)	0.3020 (13)	0.05*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Sr1	0.00824 (11)	0.00952 (13)	0.00876 (12)	0.00008 (8)	0.00180 (8)	0.00180 (9)
O1	0.0145 (8)	0.0109 (9)	0.0172 (9)	0.0003 (7)	0.0078 (7)	0.0015 (8)
O2	0.0159 (9)	0.0414 (13)	0.0193 (11)	0.0073 (9)	−0.0001 (8)	−0.0139 (9)
O3	0.0145 (8)	0.0236 (10)	0.0162 (10)	−0.0018 (8)	0.0050 (7)	0.0060 (8)
O4	0.0184 (10)	0.0565 (15)	0.0300 (13)	−0.0138 (10)	−0.0057 (9)	0.0294 (12)
O5	0.0345 (11)	0.0293 (11)	0.0111 (10)	0.0049 (9)	0.0062 (9)	−0.0023 (9)
O6	0.0125 (7)	0.0102 (8)	0.0112 (9)	−0.0020 (6)	−0.0015 (7)	−0.0015 (7)
O7	0.0195 (9)	0.0117 (9)	0.0123 (9)	0.0056 (7)	0.0028 (7)	0.0001 (7)
O8	0.0161 (8)	0.0192 (9)	0.0174 (10)	0.0049 (7)	−0.0056 (8)	−0.0093 (8)
O9	0.0125 (8)	0.0095 (8)	0.0179 (10)	−0.0005 (6)	−0.0008 (7)	0.0016 (7)
O11	0.0128 (8)	0.0093 (8)	0.0157 (9)	−0.0018 (7)	−0.0020 (7)	−0.0020 (7)
O12	0.0158 (8)	0.0052 (8)	0.0142 (9)	0.0025 (6)	0.0014 (7)	0.0023 (7)
O13	0.0286 (10)	0.0163 (9)	0.0199 (11)	−0.0104 (8)	−0.0113 (8)	0.0048 (8)
O14	0.0169 (9)	0.0069 (8)	0.0245 (11)	0.0008 (6)	−0.0003 (8)	0.0040 (7)
C6	0.0097 (10)	0.0124 (11)	0.0106 (12)	0.0029 (8)	0.0038 (9)	−0.0007 (9)
C7	0.0131 (11)	0.0132 (12)	0.0098 (12)	0.0042 (9)	0.0035 (10)	−0.0006 (10)
C8	0.0156 (11)	0.0136 (12)	0.0135 (13)	0.0038 (9)	0.0033 (10)	−0.0036 (10)
C9	0.0106 (10)	0.0093 (11)	0.0146 (12)	0.0011 (9)	0.0038 (10)	−0.0018 (10)
C11	0.0110 (10)	0.0085 (10)	0.0152 (13)	0.0003 (8)	0.0021 (10)	0.0000 (10)
C12	0.0132 (11)	0.0071 (11)	0.0142 (13)	−0.0013 (9)	0.0034 (10)	−0.0020 (10)
C13	0.0178 (12)	0.0104 (11)	0.0209 (15)	−0.0033 (9)	−0.0001 (11)	0.0031 (10)
C14	0.0121 (11)	0.0102 (11)	0.0185 (14)	−0.0014 (9)	0.0008 (10)	0.0016 (11)
O1W	0.095 (3)	0.0180 (16)	0.0227 (17)	0	0.031 (2)	0

Geometric parameters (Å, º) top

Sr1—O1	2.691 (2)	O2—H2B	0.70 (4)
Sr1—O2	2.642 (2)	O3—H3B	0.76 (4)
Sr1—O3	2.690 (2)	O3—H3A	0.93 (4)
Sr1—O4	2.641 (3)	O4—H4B	0.87 (4)
Sr1—O5	2.572 (2)	O4—H4A	0.78 (4)
Sr1—O6	2.6179 (18)	O5—H5A	0.72 (4)
Sr1—O12	2.6646 (16)	O5—H5B	0.90 (4)
Sr1—O14ⁱ	2.5906 (16)	O9—H9	0.8200
Sr1—O3ⁱⁱ	2.7154 (19)	O11—H11	0.8200
O6—C6	1.265 (3)	O1W—H1W	0.76 (2)
O7—C7	1.232 (3)	O1W—H1Wⁱⁱⁱ	0.76 (2)
O8—C8	1.231 (3)	C6—C7	1.483 (4)
O9—C9	1.310 (3)	C6—C9	1.426 (4)
O11—C11	1.311 (3)	C7—C8	1.495 (4)
O12—C12	1.262 (3)	C8—C9	1.458 (4)
O13—C13	1.225 (3)	C11—C14	1.438 (4)
O14—C14	1.244 (3)	C11—C12	1.427 (4)
O1—H1A	0.76 (4)	C12—C13	1.487 (4)
O1—H1B	0.79 (4)	C13—C14	1.495 (4)
O2—H2A	0.92 (4)

O1—Sr1—O2	128.30 (6)	Sr1—O1—H1A	112 (3)
O1—Sr1—O3	122.53 (6)	H2A—O2—H2B	117 (4)
O1—Sr1—O4	128.24 (7)	Sr1—O2—H2A	117 (2)
O1—Sr1—O5	127.55 (7)	Sr1—O2—H2B	125 (3)
O1—Sr1—O6	67.62 (6)	H3A—O3—H3B	109 (4)
O1—Sr1—O12	69.46 (5)	Sr1—O3—H3B	108 (3)
O1—Sr1—O14ⁱ	67.69 (6)	Sr1—O3—H3A	110 (3)
O1—Sr1—O3ⁱⁱ	68.26 (6)	Sr1ⁱⁱ—O3—H3A	103 (2)
O2—Sr1—O3	69.05 (6)	Sr1ⁱⁱ—O3—H3B	114 (3)
O2—Sr1—O4	103.47 (8)	Sr1—O4—H4A	115 (3)
O2—Sr1—O5	68.10 (7)	Sr1—O4—H4B	125 (2)
O2—Sr1—O6	141.02 (6)	H4A—O4—H4B	115 (4)
O2—Sr1—O12	73.90 (6)	Sr1—O5—H5A	130 (3)
O2—Sr1—O14ⁱ	138.47 (6)	Sr1—O5—H5B	120 (2)
O2—Sr1—O3ⁱⁱ	73.44 (6)	H5A—O5—H5B	108 (4)
O3—Sr1—O4	71.88 (7)	C9—O9—H9	109.00
O3—Sr1—O5	109.90 (7)	C11—O11—H11	109.00
O3—Sr1—O6	138.14 (5)	H1W—O1W—H1Wⁱⁱⁱ	120 (3)
O3—Sr1—O12	138.82 (5)	O6—C6—C7	133.8 (2)
O3—Sr1—O14ⁱ	70.92 (6)	O6—C6—C9	136.6 (2)
O3—Sr1—O3ⁱⁱ	67.95 (6)	C7—C6—C9	89.6 (2)
O4—Sr1—O5	67.68 (8)	O7—C7—C6	135.3 (2)
O4—Sr1—O6	72.28 (7)	C6—C7—C8	89.4 (2)
O4—Sr1—O12	135.59 (6)	O7—C7—C8	135.1 (2)
O4—Sr1—O14ⁱ	73.70 (7)	O8—C8—C7	134.2 (2)
O3ⁱⁱ—Sr1—O4	137.93 (7)	O8—C8—C9	137.9 (2)
O5—Sr1—O6	74.91 (7)	C7—C8—C9	87.9 (2)
O5—Sr1—O12	70.66 (7)	C6—C9—C8	93.1 (2)
O5—Sr1—O14ⁱ	138.26 (7)	O9—C9—C6	136.3 (2)
O3ⁱⁱ—Sr1—O5	138.71 (7)	O9—C9—C8	130.4 (2)
O6—Sr1—O12	82.82 (5)	C12—C11—C14	93.3 (2)
O6—Sr1—O14ⁱ	78.88 (5)	O11—C11—C12	131.6 (2)
O3ⁱⁱ—Sr1—O6	135.76 (6)	O11—C11—C14	135.1 (2)
O12—Sr1—O14ⁱ	137.07 (6)	O12—C12—C13	133.6 (2)
O3ⁱⁱ—Sr1—O12	84.97 (5)	O12—C12—C11	136.9 (2)
O3ⁱⁱ—Sr1—O14ⁱ	81.82 (5)	C11—C12—C13	89.4 (2)
Sr1—O3—Sr1ⁱⁱ	112.05 (7)	O13—C13—C12	136.0 (2)
Sr1—O6—C6	130.94 (16)	O13—C13—C14	135.3 (2)
Sr1—O12—C12	130.20 (17)	C12—C13—C14	88.6 (2)
Sr1^iv—O14—C14	134.33 (16)	O14—C14—C13	135.7 (2)
Sr1—O1—H1B	116 (3)	C11—C14—C13	88.7 (2)
H1A—O1—H1B	109 (4)	O14—C14—C11	135.5 (2)

O1—Sr1—O3—Sr1ⁱⁱ	42.91 (9)	Sr1—O6—C6—C7	−157.2 (2)
O2—Sr1—O3—Sr1ⁱⁱ	−79.97 (8)	Sr1—O6—C6—C9	26.7 (5)
O4—Sr1—O3—Sr1ⁱⁱ	167.22 (9)	Sr1—O12—C12—C11	−152.0 (3)
O5—Sr1—O3—Sr1ⁱⁱ	−135.69 (8)	Sr1—O12—C12—C13	32.5 (4)
O6—Sr1—O3—Sr1ⁱⁱ	134.93 (7)	Sr1^iv—O14—C14—C11	32.9 (5)
O12—Sr1—O3—Sr1ⁱⁱ	−52.65 (11)	Sr1^iv—O14—C14—C13	−150.9 (3)
O14ⁱ—Sr1—O3—Sr1ⁱⁱ	88.72 (7)	O6—C6—C7—O7	−2.1 (6)
O3ⁱⁱ—Sr1—O3—Sr1ⁱⁱ	0.00 (6)	O6—C6—C7—C8	−177.7 (3)
O1—Sr1—O6—C6	−106.5 (2)	C9—C6—C7—O7	175.2 (3)
O2—Sr1—O6—C6	17.3 (3)	C9—C6—C7—C8	−0.4 (2)
O3—Sr1—O6—C6	139.1 (2)	O6—C6—C9—O9	1.8 (6)
O4—Sr1—O6—C6	106.9 (2)	O6—C6—C9—C8	177.6 (3)
O5—Sr1—O6—C6	36.0 (2)	C7—C6—C9—O9	−175.3 (3)
O12—Sr1—O6—C6	−35.8 (2)	C7—C6—C9—C8	0.5 (2)
O14ⁱ—Sr1—O6—C6	−176.8 (2)	O7—C7—C8—O8	2.0 (6)
O3ⁱⁱ—Sr1—O6—C6	−111.0 (2)	O7—C7—C8—C9	−175.2 (3)
O1—Sr1—O12—C12	−112.7 (2)	C6—C7—C8—O8	177.6 (3)
O2—Sr1—O12—C12	30.1 (2)	C6—C7—C8—C9	0.4 (2)
O3—Sr1—O12—C12	3.6 (2)	O8—C8—C9—O9	−1.3 (6)
O4—Sr1—O12—C12	123.1 (2)	O8—C8—C9—C6	−177.4 (4)
O5—Sr1—O12—C12	102.0 (2)	C7—C8—C9—O9	175.7 (3)
O6—Sr1—O12—C12	178.5 (2)	C7—C8—C9—C6	−0.5 (2)
O14ⁱ—Sr1—O12—C12	−116.4 (2)	O11—C11—C12—O12	−1.5 (6)
O3ⁱⁱ—Sr1—O12—C12	−44.1 (2)	O11—C11—C12—C13	175.3 (3)
O1—Sr1—O14ⁱ—C14ⁱ	−112.4 (3)	C14—C11—C12—O12	−178.2 (3)
O2—Sr1—O14ⁱ—C14ⁱ	124.5 (2)	C14—C11—C12—C13	−1.4 (2)
O3—Sr1—O14ⁱ—C14ⁱ	108.4 (3)	O11—C11—C14—O14	2.3 (6)
O4—Sr1—O14ⁱ—C14ⁱ	32.4 (3)	O11—C11—C14—C13	−175.1 (3)
O5—Sr1—O14ⁱ—C14ⁱ	9.6 (3)	C12—C11—C14—O14	178.8 (3)
O6—Sr1—O14ⁱ—C14ⁱ	−42.2 (3)	C12—C11—C14—C13	1.4 (2)
O12—Sr1—O14ⁱ—C14ⁱ	−108.7 (2)	O12—C12—C13—O13	1.5 (6)
O1—Sr1—O3ⁱⁱ—Sr1ⁱⁱ	−141.83 (8)	O12—C12—C13—C14	178.3 (3)
O2—Sr1—O3ⁱⁱ—Sr1ⁱⁱ	73.62 (8)	C11—C12—C13—O13	−175.4 (4)
O3—Sr1—O3ⁱⁱ—Sr1ⁱⁱ	0.00 (6)	C11—C12—C13—C14	1.4 (2)
O4—Sr1—O3ⁱⁱ—Sr1ⁱⁱ	−18.28 (14)	O13—C13—C14—O14	−1.9 (6)
O5—Sr1—O3ⁱⁱ—Sr1ⁱⁱ	95.46 (11)	O13—C13—C14—C11	175.5 (4)
O6—Sr1—O3ⁱⁱ—Sr1ⁱⁱ	−137.38 (7)	C12—C13—C14—O14	−178.7 (3)
O12—Sr1—O3ⁱⁱ—Sr1ⁱⁱ	148.30 (8)	C12—C13—C14—C11	−1.4 (2)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···O9^v	0.76 (4)	2.27 (4)	2.983 (3)	158 (4)
O1—H1B···O7^vi	0.79 (4)	1.99 (4)	2.715 (2)	153 (4)
O1W—H1W···O13ⁱⁱ	0.76 (2)	2.39 (2)	2.801 (2)	115 (2)
O1W—H1W···O8^vii	0.76 (2)	2.51 (3)	3.118 (2)	138 (3)
O2—H2A···O14^viii	0.92 (4)	1.91 (4)	2.794 (3)	161 (4)
O2—H2B···O1W^iv	0.70 (4)	2.52 (4)	3.165 (3)	154 (4)
O3—H3A···O13ⁱⁱ	0.93 (4)	1.79 (4)	2.712 (3)	174 (3)
O3—H3B···O4ⁱⁱⁱ	0.76 (4)	2.59 (4)	3.172 (3)	136 (3)
O4—H4A···O7^ix	0.78 (4)	2.01 (4)	2.785 (3)	177 (4)
O4—H4B···O1W	0.87 (4)	2.03 (4)	2.871 (3)	163 (3)
O5—H5A···O1^x	0.72 (4)	2.09 (4)	2.787 (3)	166 (4)
O5—H5B···O8^xi	0.90 (4)	1.82 (4)	2.716 (3)	175 (4)
O9—H9···O12	0.82	1.74	2.548 (3)	169
O11—H11···O6^iv	0.82	1.77	2.580 (2)	172

Symmetry codes: (ii) −x+2, −y+2, −z+1; (iii) −x+2, y, −z+1/2; (iv) x, y−1, z; (v) −x+3/2, y+1/2, −z+1/2; (vi) −x+3/2, y−1/2, −z+1/2; (vii) x+1/2, −y+5/2, z+1/2; (viii) −x+2, −y+1, −z+1; (ix) −x+3/2, −y+5/2, −z; (x) x, −y+2, z−1/2; (xi) −x+3/2, −y+3/2, −z.

Experimental details

Crystal data
Chemical formula	[Sr(C₄HO₄)₂(H₂O)₅]·0.5H₂O
M_r	412.81
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	150
a, b, c (Å)	24.885 (3), 8.8026 (9), 13.8918 (17)
β (°)	119.609 (4)
V (Å³)	2645.7 (5)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	4.15
Crystal size (mm)	0.57 × 0.27 × 0.10

Data collection
Diffractometer	Bruker APEXII diffractometer
Absorption correction	Multi-scan SADABS (Bruker, 2006)
T_min, T_max	0.365, 0.660
No. of measured, independent and observed [I > 2σ(I)] reflections	9165, 3006, 2243
R_int	0.037
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.028, 0.068, 1.03
No. of reflections	3006
No. of parameters	239
No. of restraints	2
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.42, −0.51

Computer programs: APEXII (Bruker, 2006), SAINT (Bruker, 2006), SIR2002 (Burla et al., 2003), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg & Berndt, 2001), WinGX publication routines (Farrugia, 1999).

Selected bond lengths (Å) top

Sr1—O1	2.691 (2)	Sr1—O6	2.6179 (18)
Sr1—O2	2.642 (2)	Sr1—O12	2.6646 (16)
Sr1—O3	2.690 (2)	Sr1—O14ⁱ	2.5906 (16)
Sr1—O4	2.641 (3)	Sr1—O3ⁱⁱ	2.7154 (19)
Sr1—O5	2.572 (2)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···O9ⁱⁱⁱ	0.76 (4)	2.27 (4)	2.983 (3)	158 (4)
O1—H1B···O7^iv	0.79 (4)	1.99 (4)	2.715 (2)	153 (4)
O1W—H1W···O13ⁱⁱ	0.76 (2)	2.39 (2)	2.801 (2)	115 (2)
O1W—H1W···O8^v	0.76 (2)	2.51 (3)	3.118 (2)	138 (3)
O2—H2A···O14^vi	0.92 (4)	1.91 (4)	2.794 (3)	161 (4)
O2—H2B···O1W^vii	0.70 (4)	2.52 (4)	3.165 (3)	154 (4)
O3—H3A···O13ⁱⁱ	0.93 (4)	1.79 (4)	2.712 (3)	174 (3)
O3—H3B···O4^viii	0.76 (4)	2.59 (4)	3.172 (3)	136 (3)
O4—H4A···O7^ix	0.78 (4)	2.01 (4)	2.785 (3)	177 (4)
O4—H4B···O1W	0.87 (4)	2.03 (4)	2.871 (3)	163 (3)
O5—H5A···O1^x	0.72 (4)	2.09 (4)	2.787 (3)	166 (4)
O5—H5B···O8^xi	0.90 (4)	1.82 (4)	2.716 (3)	175 (4)
O9—H9···O12	0.82	1.74	2.548 (3)	169
O11—H11···O6^vii	0.82	1.77	2.580 (2)	172

Symmetry codes: (ii) −x+2, −y+2, −z+1; (iii) −x+3/2, y+1/2, −z+1/2; (iv) −x+3/2, y−1/2, −z+1/2; (v) x+1/2, −y+5/2, z+1/2; (vi) −x+2, −y+1, −z+1; (vii) x, y−1, z; (viii) −x+2, y, −z+1/2; (ix) −x+3/2, −y+5/2, −z; (x) x, −y+2, z−1/2; (xi) −x+3/2, −y+3/2, −z.

Acknowledgements

The authors thank Dr Thierry Roisnel, Centre de Diffractométrie X (CDIFX) de Rennes, Université de Rennes 1, France, for his technical assistance with the single-crystal X-ray data collection. This work was supported by the Unité de Recherche de Chimie de l'Environnement et Moléculaire Structurale, CHEMS, Université Mentouri–Constantine 25000 Algeria.

References

Brandenburg, K. & Berndt, M. (2001). DIAMOND. Crystal Impact, Bonn, Germany. Google Scholar
Bruker (2006). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103. CrossRef IUCr Journals Google Scholar
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. CrossRef IUCr Journals Google Scholar
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838. CrossRef CAS IUCr Journals Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Trifa, C., Bouhali, A., Bouacida, S., Boudaren, C. & Bataille, T. (2011). Acta Cryst. E67, m275–m276. Web of Science CSD CrossRef CAS IUCr Journals Google Scholar

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Volume 67| Part 8| August 2011| Pages m1130-m1131

doi:10.1107/S1600536811028704

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Poly[[μ-aqua-tetra­aquabis(μ-2-hy­droxy-4-oxo­cyclobut-1-ene-1,3-diolato)strontium] hemihydrate]

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Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Poly[[μ-aqua-tetraaquabis(μ-2-hydroxy-4-oxocyclobut-1-ene-1,3-diolato)strontium] hemihydrate]