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Four strontium(II) salts with organic acids have been studied. Poly[diaquadi-[mu]-ibuprofenato-strontium(II)] or poly­[diaqua­bis[[mu]-2-(4-isobutyl­phen­yl)­propionato]­strontium(II)], [Sr(C13H17O2)2(H2O)2]n, crystallizes with eight-coordinated Sr atoms. The coordination polyhedra are inter­connected by edge-sharing to form chains. The Sr coordination chains are packed into layers, which are stacked by van der Waals inter­actions. Poly[[mu]-aqua-diaquadi-[mu]-malonato-distrontium(II)], [Sr2(C3H2O4)2(H2O)3]n, crystallizes with nine-coordinated Sr atoms three-dimensionally inter­connected into a framework structure. One of the two crystallographically independent water mol­ecules is located on a twofold axial site. catena-Poly[[diaqua­(ascorbato)strontium(II)]-[mu]-ascorbato], [Sr(C6H7O6)2(H2O)2]n, crystallizes with isolated eight-coordinated Sr polyhedra. One of the ascorbate ligands bridges two Sr atoms, forming zigzag polyhedral ascorbate chains. These chains are tied together by a three-dimensional hydrogen-bonding network. Poly[aqua-[mu]-2-oxidobenzoato-strontium(II)], [Sr(C7H4O3)(H2O)]n, crystallizes with eight-coordinated Sr atoms. The polyhedra are inter­connected by face- and edge-sharing into layers. These layers are stacked by van der Waals forces between the protruding 2-oxidobenzoate ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270106005464/sk1898sup1.cif
Contains datablocks I, II, III, IV, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270106005464/sk1898Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270106005464/sk1898IIsup3.hkl
Contains datablock II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270106005464/sk1898IIIsup4.hkl
Contains datablock III

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270106005464/sk1898IVsup5.hkl
Contains datablock IV

CCDC references: 605662; 605663; 605664; 605665

Comment top

In recent years, it has been found that Sr has a significant influence on the development and growth of bone, and the effect of dose on bone structure has been investigated in great detail (Schrooten et al., 2003). These investigations have led to a growing interest in strontium(II) salts, their crystal structures and synthetic methods that may provide products of high yield and purity (Christgau et al., 2005). The present paper presents a structural investigation of four such new strontium(II) salts with organic acids.

In strontium diibuprofenate dihydrate, (I), the Sr atom is eight-coordinated in a distorted square antiprism by six O atoms from the asymmetric unit and two additional carboxylate O atoms from neighbouring ibuprofenates (O11* and O31* in Fig. 1). The ibuprofenate pair in an asymmetric unit shown in Fig. 1 have the same absolute configuration. The strontium polyhedra share edges to form chains in the a direction (Fig. 5). The chains are stacked in layers in the ab plane with the ibuprofenates protruding in the c direction. These layers are in turn stacked in the c direction, in both cases by van der Waals interactions only. Viewed in the a direction (Fig. 5), the strontium ibuprofenate complexes appear slightly tilted. This causes a difference in the packing of the two independent ibuprofenates. One ibuprofenate ion, (IA), extends further towards the next layer than the other, (IB), which is more confined to the space between the chains. This difference in packing may explain the observation of larger disorder of the terminal methyl groups of the (IA) ibuprofenate ion. The torsion angles of the isobutanyl and the propionate ends are very similar when comparing the two ibuprofenates (Table 9). Compared with the torsion angles of ibuprofen (Hansen et al., 2003), the differences in the isobutyl ends are minor, 6–8°, while the propionate ends show differences of 26–47° (Table 9). The ibuprofen conformations minimize the benzene–propionate interactions, while in (I) the coordination and packing requirements cause more strained conformations. Hydrogen bonding plays a minor role in the packing. Only one H atom of each water molecule is employed in hydrogen bonding (Table 2), and hydrogen bonding is, because of the bulkiness of the ibuprofenates, restricted to carboxylic O atoms in neighbouring strontium polyhedra within a polyhedral chain.

In strontium malonate sesquihydrate, (II), the Sr atom is nine-coordinated by all available malonate and water O atoms. The irregular polyhedra are connected by edge and face sharing into a three-dimensional framework structure. Atoms O3 and O6 are still unshared between polyhedra. The channel system thus created is occupied by the malonate carbon backbone (Fig. 6). All water H atoms are involved in hydrogen bonding to carboxylic O atoms (Table 4). By comparison, Sr malonate anhydrate (Briggman & Oskarsson, 1977) forms a similar three-dimensional polyhedral network, but all O atoms are shared between Sr polyhedra. This configuration results in a relatively dense packing, Dx = 2.78 Mg m−3, compared with 2.48 Mg m−3 in (II). The higher degree of interconnections and denser packing is the most probable cause of the irreversible dehydration of (II).

In strontium diascorbate dihydrate, (III), the Sr atom is eight-coordinated by ascorbate and water O atoms, forming isolated irregular polyhedra. The two independent ascorbate ions are coordinated differently. Ascorbate ion (IIIA) uses atoms O11, O13, O15 and O16 to coordinate two Sr ions, thus linking the Sr polyhedra into zigzagging chains in the b direction, while ascorbate ion (IIIB) has a one-sided coordination through atoms O25 and O26 (Fig. 7). The ascorbate polyhedral chains are further connected by a three-dimensional hydrogen-bonding network. The conformations of the independent ascorbate ions are different; the O14—C17—C18—C19 [for (IA)] and O24—C27—C28—C29 [for (IIIB)] torsion angles are −69.9 (2) and 176.4 (2)°, respectively. The O14—C17—C18—C19 (IIIA) torsion angle is similar to the corresponding torsion angles in ascorbic acid, −68.3 (3) and −55.5 (3)° for its two independent molecules (Hvoslef, 1968). The O15—C18—C18—O16 [(IIIA)] and O25—C28—C29—O26 [(IIIB)] torsion angles are 48.8 (2) and 50.4 (2)°, respectively, bringing them into almost eclipsed conformations and allowing for simultaneous Sr coordination of the O pairs. In ascorbic acid, the corresponding O—C—C—O torsion angles are 171.2 (3) and 171.4 (3)°, i.e. close to staggered conformations (Hvoslef, 1968). All H-atom donors are involved in hydrogen bonding, forming a three-dimensional network. It is interesting to note that the shortest hydrogen bonds (H···A < 2 Å) all involve uncoordinated O atoms from (IIIB) (Table 6), which may be explained by a higher packing/conformational flexibility of the one-sided Sr coordination of (IIIB).

In strontium 2-oxidobenzoate hydrate, (IV), the Sr atom is eight-coordinated in an approximately square antiprismatic cofiguration. The antiprisms are pair-wise connected through face-sharing, and these pairs are further connected by edge-sharing into layers in the ac plane (Fig. 8). The 2-oxidobenzoates protrude from the layers and connect them through van der Waals forces in the b direction. By comparison, the Sr disalicylate dihydrate (Debuyst et al. 1979) forms polyhedral chains, where the hydroxy group takes part in a three-dimensional hydrogen-bonding network connecting these chains. In (IV) only one of the water H-atom donors, H4B, participates in a conventional hydrogen bond. However, atom H4A points towards the center of a neighbouring benzene ring with a distance of 2.83 (3) Å to the ring center (A) and an O4—H4A···A angle of 154 (3)°.

Strontium(II) salts with organic acids are generally octa- to decacoordinated by O atoms, with coordination distances in the range 2.4–3.0 Å. The Sr polyhedra show various degrees of condensation depending on the number of available carboxylic and water O atoms, and the size of the organic group. The resulting structures are thus observed with isolated Sr polyhedra as in (III), polyhedra connected in chains as in (I), layers as in (IV) or three-dimensional networks as in (II). The average Sr—O distance is primarily determined by the coordination number as seen for (II), viz. 2.6803 (4) Å with nine-coordination, and 2.5940 (9), 2.5927 (6) and 2.6034 (7) Å for the eight-coordinated (I), (III) and (IV), respectively. An increasing degree of condensation cause a minor increase in the average Sr—O distances when comparing the eight-coordinated complexes [2.5927 (6) Å for (III), isolated; 2.5940 (9) Å for (I), chains; and 2.6034 (7) Å for (IV), layer]s.

Experimental top

For the preparation of (I), solid strontium carbonate was added to a saturated solution of racemic ibuprofen at 317 K in a molar ratio of 1:2. The product was obtained in high yield and purity after cooling to room temperature and filtration. For the preparation of (II), an equimolar amount of solid strontium carbonate was added to a saturated aqueous solution of malonic acid at 303–317 K. The product precipitated upon cooling to room temperature. Consequtive cycles of evaporation of the solvent below 343 K followed by filtration at room temperature resulted in yields between 90 and 100%. Heating of the product above 343 K resulted in complete dehydration and irreversible transformation to anhydrous strontium malonate. For the preparation of (III), strontium chloride hexahydrate was added to a solution of sodium ascorbate in a molar ratio of 1:2. More strontium chloride hexahydrate, approximately 100 g in total, and sodium ascorbate, approximately 77 g in total, were added to the solution at 317 K until a transparent yellow syrup was obtained. The syrup was suction filtered for 12 h and the product was obtained by drying the syrup in a desiccator. The final product was a white powder with a yellow tarnish, while the selected single crystals appeared colorless. The product was also obtained by pouring an aqueous solution of ascorbic acid and powdered strontium carbonate into a large volume of acetone according to the procedure of Ruskin & Merrill (1947). For the preparation of (IV), powdered strontium carbonate was added to an equimolar amount of a saturated solution of salicylic acid at 313 K. Strontium 2-oxidobenzoate hydrate was obtained in high yield and purity as a pecipitate on cooling to 293 K.

Refinement top

In all refinements all H-atom sites were initially located in difference Fourier maps and refined freely. In the final cycles, H atoms of the CH, CH2 and CH3 groups were placed in calculated positions, with C—H = 0.93 (aromatic CH), 0.98 (aliphatic CH), 0.97 (CH2) and 0.96 Å (CH3), and refined as riding atoms. In water molecules and OH groups the O—H distances were restrained to 0.82 (2) Å. The displacement parameters were set to 1.2 (CH, CH2 and CH3) or 1.5 (OH) times Ueq of the corresponding C or O atoms. In (I), several of the terminal methyl groups show signs of disorder. Several models with split positions for atoms C19, C22 and C23 were tried, with up to ten different positions. Using 353 parameters with mixed anisotrpic and isotropic displacement parameters for the different split sites, but not including the corresponding H-atom positions, resulted in an wR2 value of 0.1536, while the unsplit model including H-atom positions with 310 parameters resulted in an wR2 value of 0.1450. The unsplit model was therefore judged as appropriate on the present level of experimental resolution. The absolute structure determination of (III) is based on 2226 Bijvoet pairs.

Computing details top

For all compounds, data collection: SMART (Bruker, 1999); cell refinement: SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus and SADABS (Sheldrick, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and ATOMS (Dowty, 2000); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The asymmetric unit of (I), showing 75% probability displacement ellipsoids and the atomic numbering. H atoms have been omitted for clarity. Atoms labelled with an asterix (*) are at the symmetry positions indicated in Table 1.
[Figure 2] Fig. 2. The asymmetric unit of (II), showing 75% probability displacement ellipsoids and the atomic numbering. Atoms labelled with an asterix (*) are at the symmetry positions indicated in Table 3.
[Figure 3] Fig. 3. The asymmetric unit of (III), showing 75% probability displacement ellipsoids and the atomic numbering. Atoms labelled with an asterix (*) are at the symmetry positions indicated in Table 5.
[Figure 4] Fig. 4. The asymmetric unit of (IV), showing 75% probability displacement ellipsoids and the atomic numbering. Atoms labelled with an asterix (*) are at the symmetry positions indicated in Table 7.
[Figure 5] Fig. 5. The crystal packing of (I), viewed down the a axis. The Sr eight-coordination is shown as polyhedra. H atoms have been omitted for clarity.
[Figure 6] Fig. 6. The crystal packing of (II), viewed down the b axis. The Sr nine-coordination is shown as polyhedra. H atoms have been omitted for clarity.
[Figure 7] Fig. 7. The crystal packing of (III), viewed down the a axis. The Sr eight-coordination is shown as polyhedra. H atoms have been omitted for clarity.
[Figure 8] Fig. 8. The crystal packing of (IV), viewed down the a axis. The Sr eight-coordination is shown as polyhedra. H atoms have been omitted for clarity.
(I) poly[diaquabis[µ-2-(4-isobutylphenyl)propionato]strontium(II)] top
Crystal data top
[Sr(C13H17O2)2(H2O)2]Z = 2
Mr = 534.18F(000) = 560
Triclinic, P1Dx = 1.262 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.9116 (7) ÅCell parameters from 3382 reflections
b = 10.487 (1) Åθ = 2.3–27.6°
c = 18.2493 (17) ŵ = 1.95 mm1
α = 86.088 (2)°T = 120 K
β = 79.784 (2)°Plate, colorless
γ = 70.605 (2)°0.35 × 0.06 × 0.03 mm
V = 1405.5 (2) Å3
Data collection top
Bruker SMART APEX
diffractometer
8160 independent reflections
Radiation source: fine-focus sealed tube5038 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.051
ω scan, frame data integrationθmax = 31.0°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
h = 1111
Tmin = 0.548, Tmax = 0.944k = 1514
19139 measured reflectionsl = 2626
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.058Hydrogen site location: difference Fourier map
wR(F2) = 0.145H atoms treated by a mixture of independent and constrained refinement
S = 0.98 w = 1/[σ2(Fo2) + (0.0724P)2]
where P = (Fo2 + 2Fc2)/3
8160 reflections(Δ/σ)max = 0.001
310 parametersΔρmax = 0.79 e Å3
4 restraintsΔρmin = 0.44 e Å3
Crystal data top
[Sr(C13H17O2)2(H2O)2]γ = 70.605 (2)°
Mr = 534.18V = 1405.5 (2) Å3
Triclinic, P1Z = 2
a = 7.9116 (7) ÅMo Kα radiation
b = 10.487 (1) ŵ = 1.95 mm1
c = 18.2493 (17) ÅT = 120 K
α = 86.088 (2)°0.35 × 0.06 × 0.03 mm
β = 79.784 (2)°
Data collection top
Bruker SMART APEX
diffractometer
8160 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
5038 reflections with I > 2σ(I)
Tmin = 0.548, Tmax = 0.944Rint = 0.051
19139 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0584 restraints
wR(F2) = 0.145H atoms treated by a mixture of independent and constrained refinement
S = 0.98Δρmax = 0.79 e Å3
8160 reflectionsΔρmin = 0.44 e Å3
310 parameters
Special details top

Experimental. Oxford Cryosystem liquid nitrogen cryostream cooler

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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 > 2σ(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
xyzUiso*/Ueq
Sr10.76760 (4)0.44979 (4)0.012433 (17)0.03868 (12)
O30.8918 (3)0.3797 (3)0.13485 (14)0.0453 (6)
H310.976 (4)0.403 (4)0.139 (2)0.068*
H320.819 (5)0.400 (4)0.1733 (16)0.068*
O40.7381 (3)0.2360 (3)0.03646 (15)0.0476 (6)
H410.641 (4)0.253 (4)0.049 (2)0.071*
H420.815 (5)0.179 (3)0.065 (2)0.071*
O110.5234 (3)0.5662 (3)0.08197 (13)0.0463 (6)
O120.8107 (3)0.5425 (3)0.12268 (13)0.0464 (6)
C110.5004 (4)0.5821 (4)0.24407 (18)0.0370 (8)
C120.5251 (4)0.4451 (4)0.23561 (19)0.0405 (8)
H120.59990.39400.20290.049*
C130.4399 (5)0.3828 (4)0.27514 (18)0.0424 (8)
H130.45830.29070.26850.051*
C140.3282 (5)0.4564 (4)0.32417 (18)0.0417 (8)
C150.3020 (5)0.5935 (4)0.33199 (19)0.0427 (8)
H150.22630.64500.36430.051*
C160.3874 (5)0.6554 (4)0.29224 (18)0.0405 (8)
H160.36780.74770.29830.049*
C170.6473 (4)0.5823 (4)0.13118 (19)0.0409 (8)
C180.5944 (6)0.6549 (4)0.2032 (2)0.0534 (10)
H180.50350.74250.18840.064*
C190.7462 (8)0.6859 (7)0.2536 (3)0.110 (2)
H19A0.70350.73140.29750.132*
H19B0.84300.60320.26730.132*
H19C0.78990.74290.22830.132*
C200.2412 (7)0.3893 (5)0.3721 (2)0.0651 (12)
H20A0.11340.44140.36900.078*
H20B0.25000.29940.35260.078*
C210.3331 (10)0.3791 (6)0.4542 (2)0.094 (2)
H210.32550.47060.47240.113*
C220.2258 (13)0.3248 (8)0.4996 (3)0.177 (5)
H22A0.10130.38230.49270.212*
H22B0.23200.23480.48300.212*
H22C0.27730.32360.55140.212*
C230.5376 (11)0.2925 (6)0.4625 (3)0.129 (3)
H23A0.59840.33280.43450.155*
H23B0.59170.28870.51410.155*
H23C0.54880.20270.44390.155*
O310.8989 (3)0.6557 (3)0.02531 (13)0.0481 (6)
O320.6074 (3)0.6942 (3)0.06225 (14)0.0490 (6)
C310.8393 (4)0.8894 (3)0.12206 (17)0.0351 (7)
C320.8892 (5)1.0051 (4)0.1233 (2)0.0446 (8)
H32A0.85331.07420.08880.053*
C330.9909 (5)1.0190 (4)0.1747 (2)0.0473 (9)
H331.02301.09670.17420.057*
C341.0450 (5)0.9188 (4)0.22697 (19)0.0427 (8)
C350.9992 (5)0.8025 (3)0.22540 (18)0.0390 (8)
H351.03670.73340.25960.047*
C360.8985 (4)0.7874 (3)0.17374 (18)0.0367 (7)
H360.87010.70820.17360.044*
C370.7435 (4)0.7334 (4)0.05112 (18)0.0414 (8)
C380.7215 (5)0.8792 (4)0.0677 (2)0.0456 (9)
H380.76010.92070.02070.055*
C390.5246 (6)0.9680 (5)0.0984 (3)0.0775 (14)
H39A0.44500.96460.06500.093*
H39B0.52071.05970.10260.093*
H39C0.48620.93460.14650.093*
C401.1434 (6)0.9389 (4)0.2874 (2)0.0555 (10)
H40A1.24370.96970.26470.067*
H40B1.19340.85300.31190.067*
C411.0180 (7)1.0416 (4)0.3455 (2)0.0614 (12)
H41A0.97151.12800.31960.074*
C421.1266 (9)1.0630 (5)0.4018 (3)0.097 (2)
H42A1.22781.08830.37620.117*
H42B1.17030.98070.42940.117*
H42C1.05011.13350.43550.117*
C430.8562 (7)1.0009 (5)0.3824 (3)0.0766 (14)
H43A0.79300.98690.34490.092*
H43B0.77571.07120.41520.092*
H43C0.89730.91870.41030.092*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.01726 (14)0.0745 (3)0.03160 (17)0.02246 (14)0.00314 (11)0.01354 (14)
O30.0255 (12)0.0823 (18)0.0360 (13)0.0290 (13)0.0001 (10)0.0079 (12)
O40.0209 (12)0.0727 (18)0.0510 (16)0.0147 (12)0.0039 (11)0.0207 (13)
O110.0240 (11)0.0844 (18)0.0376 (13)0.0274 (12)0.0026 (10)0.0062 (12)
O120.0225 (11)0.0815 (17)0.0426 (14)0.0266 (12)0.0022 (10)0.0100 (12)
C110.0260 (16)0.057 (2)0.0310 (17)0.0178 (15)0.0036 (13)0.0036 (15)
C120.0287 (17)0.055 (2)0.0346 (18)0.0092 (15)0.0039 (14)0.0028 (15)
C130.049 (2)0.045 (2)0.0319 (18)0.0161 (17)0.0018 (16)0.0070 (15)
C140.0418 (19)0.055 (2)0.0307 (17)0.0202 (17)0.0005 (15)0.0120 (15)
C150.0400 (19)0.055 (2)0.0328 (18)0.0115 (17)0.0107 (15)0.0060 (15)
C160.0417 (19)0.049 (2)0.0330 (18)0.0166 (16)0.0060 (15)0.0038 (15)
C170.0302 (17)0.067 (2)0.0358 (18)0.0283 (17)0.0047 (14)0.0099 (16)
C180.053 (2)0.082 (3)0.045 (2)0.045 (2)0.0154 (18)0.0029 (19)
C190.122 (5)0.202 (7)0.066 (3)0.128 (5)0.041 (3)0.040 (4)
C200.088 (3)0.076 (3)0.049 (2)0.044 (3)0.019 (2)0.011 (2)
C210.192 (7)0.086 (4)0.041 (3)0.085 (4)0.035 (3)0.003 (2)
C220.374 (14)0.180 (7)0.071 (4)0.193 (9)0.081 (6)0.002 (4)
C230.211 (9)0.091 (4)0.060 (4)0.042 (5)0.039 (4)0.025 (3)
O310.0209 (11)0.0852 (18)0.0431 (14)0.0214 (12)0.0013 (10)0.0241 (12)
O320.0204 (11)0.0809 (18)0.0507 (15)0.0218 (11)0.0019 (10)0.0183 (13)
C310.0254 (15)0.048 (2)0.0304 (17)0.0089 (14)0.0031 (13)0.0063 (14)
C320.044 (2)0.047 (2)0.041 (2)0.0104 (17)0.0129 (16)0.0009 (16)
C330.051 (2)0.046 (2)0.048 (2)0.0170 (18)0.0087 (18)0.0104 (17)
C340.0404 (19)0.052 (2)0.0380 (19)0.0139 (16)0.0101 (16)0.0137 (16)
C350.0383 (18)0.044 (2)0.0331 (18)0.0089 (15)0.0086 (15)0.0057 (14)
C360.0330 (17)0.0432 (19)0.0351 (18)0.0123 (15)0.0053 (14)0.0104 (14)
C370.0216 (15)0.075 (2)0.0291 (17)0.0141 (16)0.0081 (13)0.0092 (16)
C380.0303 (17)0.069 (3)0.039 (2)0.0159 (17)0.0148 (15)0.0052 (17)
C390.047 (3)0.091 (3)0.096 (4)0.015 (2)0.028 (3)0.014 (3)
C400.063 (3)0.059 (2)0.052 (2)0.020 (2)0.022 (2)0.0124 (18)
C410.089 (3)0.049 (2)0.050 (2)0.020 (2)0.025 (2)0.0102 (18)
C420.166 (6)0.087 (4)0.067 (3)0.058 (4)0.054 (4)0.011 (3)
C430.096 (4)0.078 (3)0.049 (3)0.024 (3)0.002 (3)0.017 (2)
Geometric parameters (Å, º) top
Sr1—O11i2.476 (2)C22—H22A0.9600
Sr1—O31ii2.486 (2)C22—H22B0.9600
Sr1—O32.563 (3)C22—H22C0.9600
Sr1—O42.563 (3)C23—H23A0.9600
Sr1—O122.595 (2)C23—H23B0.9600
Sr1—O322.599 (3)C23—H23C0.9600
Sr1—O312.728 (2)O31—C371.257 (4)
Sr1—O112.742 (2)O32—C371.255 (4)
O3—H310.804 (18)C31—C361.393 (5)
O3—H320.815 (19)C31—C321.397 (5)
O4—H410.798 (19)C31—C381.508 (4)
O4—H420.829 (19)C32—C331.384 (5)
O11—C171.254 (4)C32—H32A0.9300
O12—C171.254 (4)C33—C341.380 (5)
C11—C161.376 (5)C33—H330.9300
C11—C121.386 (5)C34—C351.386 (5)
C11—C181.531 (5)C34—C401.520 (5)
C12—C131.390 (5)C35—C361.385 (4)
C12—H120.9300C35—H350.9300
C13—C141.382 (5)C36—H360.9300
C13—H130.9300C37—C381.526 (5)
C14—C151.385 (5)C38—C391.551 (6)
C14—C201.533 (5)C38—H380.9800
C15—C161.390 (5)C39—H39A0.9600
C15—H150.9300C39—H39B0.9600
C16—H160.9300C39—H39C0.9600
C17—C181.527 (5)C40—C411.530 (6)
C18—C191.489 (6)C40—H40A0.9700
C18—H180.9800C40—H40B0.9700
C19—H19A0.9600C41—C431.514 (6)
C19—H19B0.9600C41—C421.523 (6)
C19—H19C0.9600C41—H41A0.9800
C20—C211.540 (6)C42—H42A0.9600
C20—H20A0.9700C42—H42B0.9600
C20—H20B0.9700C42—H42C0.9600
C21—C221.537 (7)C43—H43A0.9600
C21—C231.556 (9)C43—H43B0.9600
C21—H210.9800C43—H43C0.9600
H31—O3—H32107 (4)H23B—C23—H23C109.5
H41—O4—H42109 (4)C36—C31—C32117.5 (3)
C16—C11—C12118.1 (3)C36—C31—C38122.1 (3)
C16—C11—C18118.7 (3)C32—C31—C38120.3 (3)
C12—C11—C18123.2 (3)C33—C32—C31121.3 (3)
C11—C12—C13121.1 (3)C33—C32—H32A119.3
C11—C12—H12119.4C31—C32—H32A119.3
C13—C12—H12119.4C34—C33—C32120.7 (3)
C14—C13—C12120.6 (3)C34—C33—H33119.6
C14—C13—H13119.7C32—C33—H33119.6
C12—C13—H13119.7C33—C34—C35118.4 (3)
C13—C14—C15118.2 (3)C33—C34—C40120.7 (3)
C13—C14—C20121.9 (3)C35—C34—C40120.8 (3)
C15—C14—C20119.8 (3)C36—C35—C34121.2 (3)
C14—C15—C16120.9 (3)C36—C35—H35119.4
C14—C15—H15119.5C34—C35—H35119.4
C16—C15—H15119.5C35—C36—C31120.8 (3)
C11—C16—C15121.0 (3)C35—C36—H36119.6
C11—C16—H16119.5C31—C36—H36119.6
C15—C16—H16119.5O32—C37—O31121.5 (3)
O11—C17—O12122.4 (3)O32—C37—C38119.9 (3)
O11—C17—C18118.0 (3)O31—C37—C38118.6 (3)
O12—C17—C18119.6 (3)C31—C38—C37112.8 (3)
C19—C18—C17113.9 (3)C31—C38—C39106.8 (3)
C19—C18—C11111.8 (3)C37—C38—C39114.9 (3)
C17—C18—C11112.3 (3)C31—C38—H38107.3
C19—C18—H18106.0C37—C38—H38107.3
C17—C18—H18106.0C39—C38—H38107.3
C11—C18—H18106.0C38—C39—H39A109.5
C18—C19—H19A109.5C38—C39—H39B109.5
C18—C19—H19B109.5H39A—C39—H39B109.5
H19A—C19—H19B109.5C38—C39—H39C109.5
C18—C19—H19C109.5H39A—C39—H39C109.5
H19A—C19—H19C109.5H39B—C39—H39C109.5
H19B—C19—H19C109.5C34—C40—C41112.3 (3)
C14—C20—C21112.2 (4)C34—C40—H40A109.2
C14—C20—H20A109.2C41—C40—H40A109.2
C21—C20—H20A109.2C34—C40—H40B109.2
C14—C20—H20B109.2C41—C40—H40B109.2
C21—C20—H20B109.2H40A—C40—H40B107.9
H20A—C20—H20B107.9C43—C41—C42112.2 (4)
C22—C21—C20108.8 (5)C43—C41—C40111.9 (3)
C22—C21—C23113.1 (6)C42—C41—C40109.7 (4)
C20—C21—C23111.2 (4)C43—C41—H41A107.6
C22—C21—H21107.8C42—C41—H41A107.6
C20—C21—H21107.8C40—C41—H41A107.6
C23—C21—H21107.8C41—C42—H42A109.5
C21—C22—H22A109.5C41—C42—H42B109.5
C21—C22—H22B109.5H42A—C42—H42B109.5
H22A—C22—H22B109.5C41—C42—H42C109.5
C21—C22—H22C109.5H42A—C42—H42C109.5
H22A—C22—H22C109.5H42B—C42—H42C109.5
H22B—C22—H22C109.5C41—C43—H43A109.5
C21—C23—H23A109.5C41—C43—H43B109.5
C21—C23—H23B109.5H43A—C43—H43B109.5
H23A—C23—H23B109.5C41—C43—H43C109.5
C21—C23—H23C109.5H43A—C43—H43C109.5
H23A—C23—H23C109.5H43B—C43—H43C109.5
Symmetry codes: (i) x+1, y+1, z; (ii) x+2, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H31···O12ii0.80 (2)1.92 (2)2.706 (3)165 (4)
O4—H41···O32i0.80 (2)1.91 (2)2.704 (3)171 (5)
Symmetry codes: (i) x+1, y+1, z; (ii) x+2, y+1, z.
(II) Poly[µ-aqua-diaquadi-µ-malonato-distrontium(II)] top
Crystal data top
[Sr2(C3H2O4)2(H2O)3]F(000) = 840
Mr = 433.38Dx = 2.480 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 5770 reflections
a = 14.3345 (9) Åθ = 3.0–30.9°
b = 7.3458 (5) ŵ = 9.25 mm1
c = 11.5075 (7) ÅT = 120 K
β = 106.710 (1)°Irregular, colorless
V = 1160.55 (13) Å30.33 × 0.30 × 0.08 mm
Z = 4
Data collection top
Bruker SMART APEX
diffractometer
1708 independent reflections
Radiation source: fine-focus sealed tube1630 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
ω scan, frame data integrationθmax = 30.7°, θmin = 3.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
h = 1919
Tmin = 0.06, Tmax = 0.48k = 1010
7363 measured reflectionsl = 1615
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.016H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.041 w = 1/[σ2(Fo2) + (0.0238P)2 + 0.6829P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.003
1708 reflectionsΔρmax = 0.55 e Å3
97 parametersΔρmin = 0.49 e Å3
3 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0044 (2)
Crystal data top
[Sr2(C3H2O4)2(H2O)3]V = 1160.55 (13) Å3
Mr = 433.38Z = 4
Monoclinic, C2/cMo Kα radiation
a = 14.3345 (9) ŵ = 9.25 mm1
b = 7.3458 (5) ÅT = 120 K
c = 11.5075 (7) Å0.33 × 0.30 × 0.08 mm
β = 106.710 (1)°
Data collection top
Bruker SMART APEX
diffractometer
1708 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
1630 reflections with I > 2σ(I)
Tmin = 0.06, Tmax = 0.48Rint = 0.023
7363 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0163 restraints
wR(F2) = 0.041H atoms treated by a mixture of independent and constrained refinement
S = 1.08Δρmax = 0.55 e Å3
1708 reflectionsΔρmin = 0.49 e Å3
97 parameters
Special details top

Experimental. Oxford Cryosystem liquid nitrogen cryostream cooler

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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 > 2σ(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
xyzUiso*/Ueq
Sr10.587276 (8)0.183425 (15)0.420747 (9)0.00682 (6)
O50.50000.06214 (19)0.25000.0107 (2)
H50.5347 (14)0.132 (2)0.2248 (18)0.016*
O60.55766 (7)0.53002 (14)0.39529 (9)0.01319 (19)
H6A0.5016 (11)0.551 (3)0.3629 (17)0.020*
H6B0.5791 (14)0.617 (3)0.4375 (17)0.020*
O10.59628 (7)0.26538 (14)0.20622 (8)0.01000 (18)
O20.59520 (7)0.12878 (14)0.03327 (8)0.01064 (18)
O30.88290 (7)0.24146 (14)0.35119 (8)0.01177 (18)
O40.75451 (7)0.12301 (15)0.39481 (9)0.01383 (19)
C10.63950 (10)0.18388 (15)0.13999 (12)0.0077 (2)
C20.74886 (9)0.15711 (18)0.18314 (12)0.0099 (2)
H2A0.77850.24490.14170.012*
H2B0.76340.03690.15810.012*
C30.79744 (10)0.17521 (16)0.31886 (12)0.0089 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.00625 (8)0.00896 (8)0.00554 (8)0.00000 (3)0.00218 (5)0.00040 (3)
O50.0113 (6)0.0106 (6)0.0112 (6)0.0000.0051 (5)0.000
O60.0093 (4)0.0128 (5)0.0160 (4)0.0008 (4)0.0013 (4)0.0037 (4)
O10.0095 (4)0.0130 (4)0.0084 (4)0.0018 (3)0.0039 (3)0.0006 (3)
O20.0112 (4)0.0117 (4)0.0076 (4)0.0001 (3)0.0005 (3)0.0013 (3)
O30.0088 (4)0.0161 (5)0.0098 (4)0.0022 (4)0.0017 (3)0.0016 (4)
O40.0089 (4)0.0225 (5)0.0107 (4)0.0022 (4)0.0038 (3)0.0042 (4)
C10.0071 (5)0.0077 (6)0.0080 (5)0.0011 (4)0.0018 (5)0.0016 (4)
C20.0068 (5)0.0150 (6)0.0084 (5)0.0005 (4)0.0027 (4)0.0014 (4)
C30.0082 (6)0.0094 (6)0.0092 (6)0.0021 (4)0.0023 (5)0.0007 (4)
Geometric parameters (Å, º) top
Sr1—O42.5386 (10)O6—H6A0.797 (15)
Sr1—O12.5801 (9)O6—H6B0.805 (15)
Sr1—O62.5839 (10)O1—C11.2627 (15)
Sr1—O3i2.5942 (9)O2—C11.2754 (16)
Sr1—O2ii2.6201 (10)O3—C31.2704 (16)
Sr1—O1iii2.6850 (10)O4—C31.2644 (16)
Sr1—O52.6956 (9)C1—C21.5149 (18)
Sr1—O2iii2.8423 (10)C2—C31.5219 (18)
Sr1—O4i2.9836 (11)C2—H2A0.9700
O5—H50.824 (14)C2—H2B0.9700
H6A—O6—H6B107 (2)C1—C2—H2B108.1
O1—C1—O2122.46 (12)C3—C2—H2B108.1
O1—C1—C2120.31 (11)H2A—C2—H2B107.3
O2—C1—C2117.14 (11)O4—C3—O3122.25 (12)
C1—C2—C3116.75 (10)O4—C3—C2120.85 (12)
C1—C2—H2A108.1O3—C3—C2116.88 (11)
C3—C2—H2A108.1
Symmetry codes: (i) x+3/2, y+1/2, z+1; (ii) x, y, z+1/2; (iii) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5···O3iv0.82 (1)1.90 (1)2.7165 (12)170 (2)
O6—H6A···O3v0.80 (2)2.18 (2)2.8662 (14)145 (2)
O6—H6B···O2vi0.81 (2)2.15 (2)2.9328 (14)164 (2)
Symmetry codes: (iv) x+3/2, y1/2, z+1/2; (v) x1/2, y+1/2, z; (vi) x, y+1, z+1/2.
(III) catena-Poly[[diaqua(ascorbato)strontium(II)]-µ-ascorbato] top
Crystal data top
[Sr(C6H7O6)2(H2O)2]F(000) = 480
Mr = 473.88Dx = 1.906 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ybCell parameters from 6673 reflections
a = 6.4358 (5) Åθ = 2.5–30.7°
b = 16.1040 (13) ŵ = 3.34 mm1
c = 8.3646 (7) ÅT = 120 K
β = 107.696 (1)°Irregular, colorless
V = 825.90 (12) Å30.28 × 0.05 × 0.04 mm
Z = 2
Data collection top
Bruker SMART APEX
diffractometer
4728 independent reflections
Radiation source: fine-focus sealed tube4507 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
ω scan, frame data integrationθmax = 30.9°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
h = 99
Tmin = 0.455, Tmax = 0.878k = 2223
10978 measured reflectionsl = 1211
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.057 w = 1/[σ2(Fo2) + (0.0321P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
4728 reflectionsΔρmax = 0.73 e Å3
274 parametersΔρmin = 0.28 e Å3
11 restraintsAbsolute structure: Flack (1983), 2035 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.017 (4)
Crystal data top
[Sr(C6H7O6)2(H2O)2]V = 825.90 (12) Å3
Mr = 473.88Z = 2
Monoclinic, P21Mo Kα radiation
a = 6.4358 (5) ŵ = 3.34 mm1
b = 16.1040 (13) ÅT = 120 K
c = 8.3646 (7) Å0.28 × 0.05 × 0.04 mm
β = 107.696 (1)°
Data collection top
Bruker SMART APEX
diffractometer
4728 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
4507 reflections with I > 2σ(I)
Tmin = 0.455, Tmax = 0.878Rint = 0.023
10978 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.025H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.057Δρmax = 0.73 e Å3
S = 1.04Δρmin = 0.28 e Å3
4728 reflectionsAbsolute structure: Flack (1983), 2035 Friedel pairs
274 parametersAbsolute structure parameter: 0.017 (4)
11 restraints
Special details top

Experimental. Oxford Cryosystem liquid nitrogen cryostream cooler

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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 > 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
xyzUiso*/Ueq
Sr10.02286 (3)0.889795 (13)0.77741 (2)0.00880 (5)
O10.3373 (3)0.87790 (10)0.5303 (2)0.0173 (3)
H1A0.367 (5)0.8328 (14)0.481 (4)0.026*
H1B0.353 (5)0.9149 (15)0.464 (3)0.026*
O20.4158 (3)0.84918 (11)0.9468 (2)0.0178 (3)
H2A0.456 (5)0.8027 (13)0.983 (4)0.027*
H2B0.530 (3)0.8693 (18)0.946 (4)0.027*
O110.1618 (3)0.78079 (10)0.9079 (2)0.0133 (3)
O120.4119 (3)0.68869 (10)1.08944 (19)0.0119 (3)
H120.411 (5)0.6975 (18)1.186 (2)0.018*
O130.0986 (3)0.54439 (9)1.2563 (2)0.0117 (3)
O140.0906 (2)0.67923 (9)0.98560 (18)0.0109 (3)
O150.2856 (3)0.47033 (9)1.13780 (19)0.0114 (3)
H150.381 (4)0.4895 (18)1.212 (3)0.017*
O160.1178 (3)0.45095 (11)0.9253 (2)0.0146 (3)
H160.242 (3)0.4591 (19)0.871 (3)0.022*
C140.1049 (3)0.71517 (13)0.9845 (3)0.0090 (4)
C150.2095 (3)0.66672 (13)1.0807 (2)0.0094 (4)
C160.0767 (3)0.60100 (13)1.1513 (2)0.0094 (4)
C170.1305 (3)0.60872 (12)1.0993 (3)0.0095 (4)
H170.24990.62381.19950.011*
C180.2082 (4)0.53544 (13)1.0153 (3)0.0102 (4)
H180.33020.55420.97730.012*
C190.0354 (4)0.49712 (14)0.8664 (3)0.0134 (4)
H19A0.04010.54060.79050.016*
H19B0.10450.46060.80540.016*
O210.4790 (2)0.49852 (11)0.70847 (19)0.0145 (3)
O220.6075 (3)0.53606 (10)0.4076 (2)0.0123 (3)
H220.704 (4)0.5523 (18)0.377 (4)0.018*
O230.5624 (3)0.72781 (10)0.3809 (2)0.0124 (3)
O240.4032 (3)0.63437 (9)0.71404 (18)0.0128 (3)
O250.0576 (3)0.74240 (10)0.6550 (2)0.0130 (3)
H250.093 (5)0.7074 (15)0.723 (3)0.020*
O260.1785 (3)0.87959 (11)0.52356 (19)0.0144 (3)
H260.296 (3)0.891 (2)0.521 (3)0.022*
C240.4774 (4)0.56818 (15)0.6452 (3)0.0106 (4)
C250.5420 (4)0.59363 (14)0.5032 (3)0.0094 (4)
C260.5169 (4)0.67820 (14)0.4846 (3)0.0097 (4)
C270.4051 (4)0.70724 (13)0.6114 (3)0.0098 (4)
H270.48400.75350.67940.012*
C280.1622 (4)0.72909 (13)0.5272 (3)0.0110 (4)
H280.09120.68220.45700.013*
C290.1212 (4)0.80711 (14)0.4207 (3)0.0135 (4)
H29A0.20670.80520.34320.016*
H29B0.03160.80980.35550.016*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.01028 (8)0.00692 (7)0.01035 (7)0.00003 (9)0.00486 (5)0.00059 (9)
O10.0248 (8)0.0091 (9)0.0153 (7)0.0008 (7)0.0022 (6)0.0014 (6)
O20.0113 (8)0.0183 (8)0.0243 (9)0.0027 (7)0.0060 (7)0.0035 (7)
O110.0161 (8)0.0099 (7)0.0156 (7)0.0030 (6)0.0075 (6)0.0035 (6)
O120.0107 (7)0.0156 (7)0.0109 (7)0.0025 (6)0.0056 (6)0.0002 (6)
O130.0166 (8)0.0079 (7)0.0142 (7)0.0007 (6)0.0098 (6)0.0021 (6)
O140.0118 (7)0.0089 (7)0.0142 (7)0.0011 (6)0.0072 (6)0.0042 (6)
O150.0118 (7)0.0090 (7)0.0119 (7)0.0002 (6)0.0017 (6)0.0011 (6)
O160.0108 (7)0.0184 (8)0.0134 (7)0.0035 (6)0.0016 (6)0.0033 (6)
C140.0098 (9)0.0083 (9)0.0096 (9)0.0018 (8)0.0040 (7)0.0013 (7)
C150.0096 (9)0.0105 (9)0.0096 (9)0.0003 (7)0.0051 (7)0.0001 (7)
C160.0122 (9)0.0078 (9)0.0086 (9)0.0013 (8)0.0039 (7)0.0014 (7)
C170.0110 (9)0.0060 (9)0.0117 (9)0.0003 (7)0.0036 (7)0.0027 (7)
C180.0124 (10)0.0093 (9)0.0100 (9)0.0018 (8)0.0051 (8)0.0003 (7)
C190.0153 (10)0.0156 (10)0.0109 (10)0.0027 (9)0.0063 (8)0.0004 (8)
O210.0170 (8)0.0133 (8)0.0139 (8)0.0010 (6)0.0056 (6)0.0030 (6)
O220.0158 (8)0.0088 (7)0.0167 (8)0.0003 (6)0.0114 (6)0.0028 (6)
O230.0166 (9)0.0110 (8)0.0118 (7)0.0020 (6)0.0076 (6)0.0008 (6)
O240.0190 (8)0.0107 (7)0.0104 (7)0.0018 (6)0.0072 (6)0.0014 (5)
O250.0190 (8)0.0099 (7)0.0145 (8)0.0008 (6)0.0116 (7)0.0007 (6)
O260.0189 (7)0.0089 (8)0.0187 (7)0.0028 (7)0.0107 (6)0.0022 (6)
C240.0093 (10)0.0116 (10)0.0101 (10)0.0010 (8)0.0018 (8)0.0011 (8)
C250.0084 (10)0.0100 (10)0.0109 (9)0.0009 (8)0.0047 (8)0.0018 (8)
C260.0074 (10)0.0124 (10)0.0100 (9)0.0004 (8)0.0035 (8)0.0039 (7)
C270.0137 (10)0.0070 (9)0.0101 (9)0.0007 (8)0.0057 (8)0.0002 (8)
C280.0136 (10)0.0112 (9)0.0099 (9)0.0008 (8)0.0060 (8)0.0016 (7)
C290.0159 (10)0.0143 (10)0.0111 (9)0.0033 (8)0.0054 (8)0.0001 (8)
Geometric parameters (Å, º) top
Sr1—O112.5446 (16)C17—C181.533 (3)
Sr1—O13i2.5688 (15)C17—H170.9800
Sr1—O16i2.5699 (16)C18—C191.525 (3)
Sr1—O22.5790 (17)C18—H180.9800
Sr1—O12.6016 (16)C19—H19A0.9700
Sr1—O262.6138 (15)C19—H19B0.9700
Sr1—O252.6215 (16)O21—C241.239 (3)
Sr1—O15i2.6423 (16)O22—C251.372 (3)
O1—H1A0.829 (18)O22—H220.782 (17)
O1—H1B0.797 (17)O23—C261.277 (3)
O2—H2A0.820 (17)O24—C241.365 (3)
O2—H2B0.804 (17)O24—C271.456 (3)
O11—C141.232 (3)O25—C281.442 (3)
O12—C151.373 (3)O25—H250.783 (17)
O12—H120.821 (17)O26—C291.430 (3)
O13—C161.302 (2)O26—H260.785 (17)
O14—C141.383 (3)C24—C251.432 (3)
O14—C171.453 (2)C25—C261.375 (3)
O15—C181.445 (2)C26—C271.525 (3)
O15—H150.791 (17)C27—C281.547 (3)
O16—C191.437 (3)C27—H270.9800
O16—H160.802 (18)C28—C291.516 (3)
C14—C151.427 (3)C28—H280.9800
C15—C161.376 (3)C29—H29A0.9700
C16—C171.528 (3)C29—H29B0.9700
H1A—O1—H1B110 (3)H19A—C19—H19B108.2
H2A—O2—H2B101 (3)C25—O22—H22112 (2)
C15—O12—H12112 (2)C24—O24—C27108.30 (16)
C14—O14—C17108.08 (15)C28—O25—H25109 (2)
C18—O15—H15107 (2)C29—O26—H26105 (3)
C19—O16—H16113 (2)O21—C24—O24119.0 (2)
O11—C14—O14119.23 (18)O21—C24—C25130.3 (2)
O11—C14—C15130.2 (2)O24—C24—C25110.7 (2)
O14—C14—C15110.58 (17)O22—C25—C26130.5 (2)
O12—C15—C16130.59 (19)O22—C25—C24120.5 (2)
O12—C15—C14120.43 (18)C26—C25—C24108.9 (2)
C16—C15—C14108.97 (19)O23—C26—C25130.8 (2)
O13—C16—C15130.36 (19)O23—C26—C27122.3 (2)
O13—C16—C17122.10 (18)C25—C26—C27106.82 (19)
C15—C16—C17107.27 (17)O24—C27—C26104.65 (17)
O14—C17—C16104.74 (16)O24—C27—C28105.29 (17)
O14—C17—C18108.56 (15)C26—C27—C28112.24 (18)
C16—C17—C18120.17 (17)O24—C27—H27111.4
O14—C17—H17107.6C26—C27—H27111.4
C16—C17—H17107.6C28—C27—H27111.4
C18—C17—H17107.6O25—C28—C29105.96 (17)
O15—C18—C19107.10 (17)O25—C28—C27109.34 (17)
O15—C18—C17108.88 (16)C29—C28—C27115.30 (18)
C19—C18—C17115.30 (18)O25—C28—H28108.7
O15—C18—H18108.5C29—C28—H28108.7
C19—C18—H18108.5C27—C28—H28108.7
C17—C18—H18108.5O26—C29—C28110.87 (17)
O16—C19—C18109.59 (17)O26—C29—H29A109.5
O16—C19—H19A109.8C28—C29—H29A109.5
C18—C19—H19A109.8O26—C29—H29B109.5
O16—C19—H19B109.8C28—C29—H29B109.5
C18—C19—H19B109.8H29A—C29—H29B108.1
Symmetry code: (i) x, y+1/2, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O23ii0.83 (2)1.88 (2)2.708 (2)177 (3)
O1—H1B···O21iii0.80 (2)1.96 (2)2.736 (2)163 (3)
O2—H2A···O12iv0.82 (2)2.10 (2)2.920 (2)175 (3)
O2—H2B···O15v0.80 (2)2.25 (2)2.971 (2)150 (3)
O12—H12···O23vi0.82 (2)1.76 (2)2.571 (2)172 (3)
O15—H15···O22vii0.79 (2)1.98 (2)2.768 (2)177 (3)
O16—H16···O21ii0.80 (2)2.00 (2)2.783 (2)167 (3)
O22—H22···O13viii0.78 (2)1.86 (2)2.579 (2)154 (3)
O25—H25···O140.78 (2)2.25 (2)2.893 (2)140 (3)
O26—H26···O1iv0.79 (2)2.35 (2)3.100 (2)161 (4)
Symmetry codes: (ii) x1, y, z; (iii) x, y+1/2, z+1; (iv) x+1, y, z; (v) x+1, y+1/2, z+2; (vi) x1, y, z+1; (vii) x, y, z+1; (viii) x+1, y, z1.
(IV) Poly[aqua-µ-2-oxidobenzoato-strontium(II)] top
Crystal data top
[Sr(C7H4O3)(H2O)]F(000) = 472
Mr = 241.74Dx = 2.101 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 4077 reflections
a = 5.0993 (4) Åθ = 3.2–30.4°
b = 22.808 (2) ŵ = 7.02 mm1
c = 6.9811 (6) ÅT = 120 K
β = 109.755 (2)°Irregular, colorless
V = 764.15 (11) Å30.14 × 0.10 × 0.02 mm
Z = 4
Data collection top
Bruker SMART APEX
diffractometer
2251 independent reflections
Radiation source: fine-focus sealed tube1917 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
ω scan, frame data integrationθmax = 30.9°, θmin = 3.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
h = 77
Tmin = 0.440, Tmax = 0.872k = 3232
10002 measured reflectionsl = 910
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038Hydrogen site location: difference Fourier map
wR(F2) = 0.092H atoms treated by a mixture of independent and constrained refinement
S = 1.08 w = 1/[σ2(Fo2) + (0.0573P)2 + 0.1094P]
where P = (Fo2 + 2Fc2)/3
2251 reflections(Δ/σ)max < 0.001
115 parametersΔρmax = 1.87 e Å3
2 restraintsΔρmin = 1.00 e Å3
Crystal data top
[Sr(C7H4O3)(H2O)]V = 764.15 (11) Å3
Mr = 241.74Z = 4
Monoclinic, P21/nMo Kα radiation
a = 5.0993 (4) ŵ = 7.02 mm1
b = 22.808 (2) ÅT = 120 K
c = 6.9811 (6) Å0.14 × 0.10 × 0.02 mm
β = 109.755 (2)°
Data collection top
Bruker SMART APEX
diffractometer
2251 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
1917 reflections with I > 2σ(I)
Tmin = 0.440, Tmax = 0.872Rint = 0.040
10002 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0382 restraints
wR(F2) = 0.092H atoms treated by a mixture of independent and constrained refinement
S = 1.08Δρmax = 1.87 e Å3
2251 reflectionsΔρmin = 1.00 e Å3
115 parameters
Special details top

Experimental. Oxford Cryosystem liquid nitrogen cryostream cooler

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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 > 2σ(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
xyzUiso*/Ueq
Sr10.21082 (5)0.023582 (11)0.79827 (4)0.00859 (10)
O10.1711 (4)0.04870 (9)0.4455 (3)0.0124 (4)
O20.2722 (4)0.01515 (9)0.1812 (3)0.0116 (4)
O30.6267 (4)0.07957 (8)0.0468 (3)0.0110 (4)
C10.4460 (6)0.11029 (12)0.3122 (4)0.0101 (5)
C20.6007 (6)0.11929 (12)0.1780 (4)0.0103 (5)
C30.7369 (6)0.17410 (13)0.1914 (5)0.0156 (6)
H30.83770.18140.10500.019*
C40.7254 (7)0.21696 (14)0.3274 (5)0.0192 (7)
H40.81880.25220.33200.023*
C50.5744 (7)0.20779 (13)0.4587 (5)0.0162 (6)
H50.56790.23650.55170.019*
C60.4350 (6)0.15527 (13)0.4476 (5)0.0134 (6)
H60.33040.14940.53230.016*
C70.2914 (6)0.05545 (13)0.3132 (4)0.0107 (5)
O40.0506 (5)0.11408 (9)0.8271 (4)0.0169 (4)
H4A0.148 (7)0.1349 (16)0.734 (5)0.025*
H4B0.164 (7)0.1041 (17)0.881 (6)0.025*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.00914 (15)0.01337 (15)0.00278 (14)0.00060 (9)0.00138 (10)0.00005 (8)
O10.0150 (10)0.0183 (10)0.0049 (9)0.0021 (8)0.0048 (8)0.0000 (8)
O20.0127 (10)0.0143 (10)0.0070 (10)0.0019 (7)0.0024 (8)0.0025 (7)
O30.0114 (10)0.0141 (9)0.0080 (10)0.0013 (7)0.0040 (8)0.0015 (7)
C10.0100 (12)0.0135 (12)0.0061 (12)0.0003 (10)0.0017 (10)0.0003 (10)
C20.0106 (12)0.0131 (12)0.0063 (12)0.0009 (10)0.0017 (10)0.0007 (10)
C30.0159 (14)0.0154 (14)0.0189 (16)0.0031 (11)0.0102 (13)0.0013 (11)
C40.0229 (16)0.0149 (14)0.0189 (16)0.0032 (11)0.0059 (14)0.0023 (12)
C50.0177 (15)0.0154 (14)0.0142 (15)0.0030 (11)0.0039 (12)0.0029 (11)
C60.0140 (13)0.0177 (14)0.0093 (13)0.0011 (10)0.0049 (11)0.0022 (10)
C70.0091 (12)0.0162 (13)0.0055 (13)0.0015 (10)0.0007 (10)0.0033 (9)
O40.0174 (11)0.0196 (11)0.0153 (11)0.0018 (9)0.0077 (9)0.0041 (9)
Geometric parameters (Å, º) top
Sr1—O12.469 (2)C1—C21.429 (4)
Sr1—O42.502 (2)C1—C71.480 (4)
Sr1—O3i2.579 (2)C2—C31.418 (4)
Sr1—O2i2.591 (2)C3—C41.378 (4)
Sr1—O3ii2.605 (2)C3—H30.9300
Sr1—O2iii2.666 (2)C4—C51.398 (4)
Sr1—O1iii2.677 (2)C4—H40.9300
Sr1—O2ii2.738 (2)C5—C61.382 (4)
O1—C71.279 (3)C5—H50.9300
O2—C71.282 (3)C6—H60.9300
O3—C21.326 (3)O4—H4A0.821 (19)
C1—C61.409 (4)O4—H4B0.823 (18)
C6—C1—C2119.4 (3)C5—C4—H4119.8
C6—C1—C7118.0 (2)C6—C5—C4118.7 (3)
C2—C1—C7122.5 (2)C6—C5—H5120.7
O3—C2—C3119.1 (2)C4—C5—H5120.7
O3—C2—C1124.1 (2)C5—C6—C1122.2 (3)
C3—C2—C1116.7 (3)C5—C6—H6118.9
C4—C3—C2122.5 (3)C1—C6—H6118.9
C4—C3—H3118.8O1—C7—O2119.6 (3)
C2—C3—H3118.8O1—C7—C1119.4 (3)
C3—C4—C5120.5 (3)O2—C7—C1120.9 (2)
C3—C4—H4119.8H4A—O4—H4B101 (4)
Symmetry codes: (i) x, y, z+1; (ii) x+1, y, z+1; (iii) x, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O4—H4B···O3iv0.82 (2)1.90 (2)2.718 (3)170 (4)
Symmetry code: (iv) x1, y, z+1.

Experimental details

(I)(II)(III)(IV)
Crystal data
Chemical formula[Sr(C13H17O2)2(H2O)2][Sr2(C3H2O4)2(H2O)3][Sr(C6H7O6)2(H2O)2][Sr(C7H4O3)(H2O)]
Mr534.18433.38473.88241.74
Crystal system, space groupTriclinic, P1Monoclinic, C2/cMonoclinic, P21Monoclinic, P21/n
Temperature (K)120120120120
a, b, c (Å)7.9116 (7), 10.487 (1), 18.2493 (17)14.3345 (9), 7.3458 (5), 11.5075 (7)6.4358 (5), 16.1040 (13), 8.3646 (7)5.0993 (4), 22.808 (2), 6.9811 (6)
α, β, γ (°)86.088 (2), 79.784 (2), 70.605 (2)90, 106.710 (1), 9090, 107.696 (1), 9090, 109.755 (2), 90
V3)1405.5 (2)1160.55 (13)825.90 (12)764.15 (11)
Z2424
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)1.959.253.347.02
Crystal size (mm)0.35 × 0.06 × 0.030.33 × 0.30 × 0.080.28 × 0.05 × 0.040.14 × 0.10 × 0.02
Data collection
DiffractometerBruker SMART APEX
diffractometer
Bruker SMART APEX
diffractometer
Bruker SMART APEX
diffractometer
Bruker SMART APEX
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2002)
Multi-scan
(SADABS; Sheldrick, 2002)
Multi-scan
(SADABS; Sheldrick, 2002)
Multi-scan
(SADABS; Sheldrick, 2002)
Tmin, Tmax0.548, 0.9440.06, 0.480.455, 0.8780.440, 0.872
No. of measured, independent and
observed [I > 2σ(I)] reflections
19139, 8160, 5038 7363, 1708, 1630 10978, 4728, 4507 10002, 2251, 1917
Rint0.0510.0230.0230.040
(sin θ/λ)max1)0.7250.7190.7230.721
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.058, 0.145, 0.98 0.016, 0.041, 1.08 0.025, 0.057, 1.04 0.038, 0.092, 1.08
No. of reflections8160170847282251
No. of parameters31097274115
No. of restraints43112
H-atom treatmentH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.79, 0.440.55, 0.490.73, 0.281.87, 1.00
Absolute structure??Flack (1983), 2035 Friedel pairs?
Absolute structure parameter??0.017 (4)?

Computer programs: SMART (Bruker, 1999), SAINT-Plus (Bruker, 1999), SAINT-Plus and SADABS (Sheldrick, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997) and ATOMS (Dowty, 2000), SHELXL97.

Selected bond lengths (Å) for (I) top
Sr1—O11i2.476 (2)Sr1—O122.595 (2)
Sr1—O31ii2.486 (2)Sr1—O322.599 (3)
Sr1—O32.563 (3)Sr1—O312.728 (2)
Sr1—O42.563 (3)Sr1—O112.742 (2)
Symmetry codes: (i) x+1, y+1, z; (ii) x+2, y+1, z.
Hydrogen-bond geometry (Å, º) for (I) top
D—H···AD—HH···AD···AD—H···A
O3—H31···O12ii0.804 (18)1.92 (2)2.706 (3)165 (4)
O4—H41···O32i0.798 (19)1.91 (2)2.704 (3)171 (5)
Symmetry codes: (i) x+1, y+1, z; (ii) x+2, y+1, z.
Selected bond lengths (Å) for (II) top
Sr1—O42.5386 (10)Sr1—O1iii2.6850 (10)
Sr1—O12.5801 (9)Sr1—O52.6956 (9)
Sr1—O62.5839 (10)Sr1—O2iii2.8423 (10)
Sr1—O3i2.5942 (9)Sr1—O4i2.9836 (11)
Sr1—O2ii2.6201 (10)
Symmetry codes: (i) x+3/2, y+1/2, z+1; (ii) x, y, z+1/2; (iii) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) for (II) top
D—H···AD—HH···AD···AD—H···A
O5—H5···O3iv0.824 (14)1.902 (14)2.7165 (12)169.7 (19)
O6—H6A···O3v0.797 (15)2.179 (17)2.8662 (14)144.6 (19)
O6—H6B···O2vi0.805 (15)2.150 (16)2.9328 (14)164.2 (19)
Symmetry codes: (iv) x+3/2, y1/2, z+1/2; (v) x1/2, y+1/2, z; (vi) x, y+1, z+1/2.
Selected bond lengths (Å) for (III) top
Sr1—O112.5446 (16)Sr1—O22.5790 (17)
Sr1—O13i2.5688 (15)Sr1—O12.6016 (16)
Sr1—O16i2.5699 (16)
Symmetry code: (i) x, y+1/2, z+2.
Hydrogen-bond geometry (Å, º) for (III) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O23ii0.829 (18)1.879 (18)2.708 (2)177 (3)
O1—H1B···O21iii0.797 (17)1.963 (19)2.736 (2)163 (3)
O2—H2A···O12iv0.820 (17)2.104 (18)2.920 (2)175 (3)
O2—H2B···O15v0.804 (17)2.25 (2)2.971 (2)150 (3)
O12—H12···O23vi0.821 (17)1.756 (18)2.571 (2)172 (3)
O15—H15···O22vii0.791 (17)1.978 (17)2.768 (2)177 (3)
O16—H16···O21ii0.802 (18)1.997 (19)2.783 (2)167 (3)
O22—H22···O13viii0.782 (17)1.86 (2)2.579 (2)154 (3)
O25—H25···O140.783 (17)2.25 (2)2.893 (2)140 (3)
O26—H26···O1iv0.785 (17)2.348 (19)3.100 (2)161 (4)
Symmetry codes: (ii) x1, y, z; (iii) x, y+1/2, z+1; (iv) x+1, y, z; (v) x+1, y+1/2, z+2; (vi) x1, y, z+1; (vii) x, y, z+1; (viii) x+1, y, z1.
Selected bond lengths (Å) for (IV) top
Sr1—O12.469 (2)Sr1—O3ii2.605 (2)
Sr1—O42.502 (2)Sr1—O2iii2.666 (2)
Sr1—O3i2.579 (2)Sr1—O1iii2.677 (2)
Sr1—O2i2.591 (2)Sr1—O2ii2.738 (2)
Symmetry codes: (i) x, y, z+1; (ii) x+1, y, z+1; (iii) x, y, z+1.
Hydrogen-bond geometry (Å, º) for (IV) top
D—H···AD—HH···AD···AD—H···A
O4—H4B···O3iv0.823 (18)1.90 (2)2.718 (3)170 (4)
Symmetry code: (iv) x1, y, z+1.
Selected torsion angles in (I) (°) top
(I)Ibuprofena
C14—C20—C21—C22-174.1 (5)-168.3 (5)
C34—C40—C41—C42-176.9 (4)168.7 (5)
C12—C11—C18—C19104.8 (5)144.4 (4)
C36—C31—C38—C39101.9 (4)151.2 (4)
C11—C18—C17—O11-59.6 (5)-95.9 (4)
C31—C38—C37—O31-58.0 (4)-83.6 (4)
Note: (a) Hansen et al. (2003).
 

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