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

In the title coordination polymer, {[Sr(C(4)HO(4))(2)(H(2)O)(5)]·0.5H(2)O}(n), the Sr(2+) ion is coordinated by three monodentate hydrogensquarate (hsq) anions and six aqua ligands in a distorted SrO(9) monocapped square-anti-prismatic geometry. The hsq anions and water mol-ecules bridge the metal ions into infinite sheets lying parallel to (100). The O atom of the uncoordinated water mol-ecule 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 = 412.81

Monoclinic,

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[F 2 > 2σ(F 2)] = 0.028

wR(F 2) = 0.068

S = 1.03

3006 reflections

239 parameters

2 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.42 e Å−3

Δρmin = −0.51 e Å−3

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 ▶).

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811028704/hb5939sup1.cif

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

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Sr(C4HO4)2(H2O)5]·0.5H2O	F(000) = 1656
Mr = 412.81	Dx = 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

Bruker APEXII diffractometer	2243 reflections with I > 2σ(I)
graphite	Rint = 0.037
CCD rotation images, thin slices scans	θmax = 27.5°, θmin = 2.7°
Absorption correction: multi-scan SADABS (Bruker, 2006)	h = −32→32
Tmin = 0.365, Tmax = 0.660	k = −8→11
9165 measured reflections	l = −17→18
3006 independent reflections

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(Fo2) + (0.0273P)2 + 1.5645P] where P = (Fo2 + 2Fc2)/3
3006 reflections	(Δ/σ)max = 0.001
239 parameters	Δρmax = 0.42 e Å−3
2 restraints	Δρmin = −0.51 e Å−3

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.

	x	y	z	Uiso*/Ueq
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*

	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

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)
Sr1iv—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)	Sr1iv—O14—C14—C11	32.9 (5)
O12—Sr1—O3—Sr1ii	−52.65 (11)	Sr1iv—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)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···O9v	0.76 (4)	2.27 (4)	2.983 (3)	158 (4)
O1—H1B···O7vi	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···O8vii	0.76 (2)	2.51 (3)	3.118 (2)	138 (3)
O2—H2A···O14viii	0.92 (4)	1.91 (4)	2.794 (3)	161 (4)
O2—H2B···O1Wiv	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···O7ix	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···O1x	0.72 (4)	2.09 (4)	2.787 (3)	166 (4)
O5—H5B···O8xi	0.90 (4)	1.82 (4)	2.716 (3)	175 (4)
O9—H9···O12	0.82	1.74	2.548 (3)	169
O11—H11···O6iv	0.82	1.77	2.580 (2)	172

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) ; (ii) .

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⋯O7iv	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⋯O8v	0.76 (2)	2.51 (3)	3.118 (2)	138 (3)
O2—H2A⋯O14vi	0.92 (4)	1.91 (4)	2.794 (3)	161 (4)
O2—H2B⋯O1Wvii	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⋯O4viii	0.76 (4)	2.59 (4)	3.172 (3)	136 (3)
O4—H4A⋯O7ix	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⋯O1x	0.72 (4)	2.09 (4)	2.787 (3)	166 (4)
O5—H5B⋯O8xi	0.90 (4)	1.82 (4)	2.716 (3)	175 (4)
O9—H9⋯O12	0.82	1.74	2.548 (3)	169
O11—H11⋯O6vii	0.82	1.77	2.580 (2)	172

Symmetry codes: (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) ; (x) ; (xi) .