Poly[[tetra­aqua­tris(monomethyl fumarato)­distrontium(II)] monomethyl fumarate] at 120 K

The title compound, {[Sr₂(C₅H₅O₄)₃(H₂O)₄](C₅H₅O₄)}_n, crystallizes with three methyl fumarate ions and four water mol­ecules coordinating the two independent strontium(II) ions. The coordination polyhedra are inter­connected by edge-sharing to form chains, which are connected by hydrogen bonds into layers. The layers, in turn, are stacked with the fourth methyl fumarate anion intercalated.

Key indicators

• Single-crystal X-ray study
• T = 120 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.038
• wR factor = 0.095
• Data-to-parameter ratio = 20.7

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.08
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       2.51 Ratio
PLAT731_ALERT_1_C Bond    Calc     0.81(4), Rep   0.809(18) ......       2.22 su-Rat
              O2   -H2A     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.80(4), Rep   0.792(18) ......       2.22 su-Rat
              O3   -H3B     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.81(4), Rep   0.807(18) ......       2.22 su-Rat
              O4   -H4B     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.81(4), Rep   0.809(18) ......       2.22 su-Rat
              O2   -H2A     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.80(4), Rep   0.792(18) ......       2.22 su-Rat
              O3   -H3B     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.81(4), Rep   0.807(18) ......       2.22 su-Rat
              O4   -H4B     1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     2.01(4), Rep   2.017(19) ......       2.11 su-Rat
              H2A  -O21     1.555   2.666

Alert level G
FORMU01_ALERT_1_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety. This is
            usually due to the moiety formula being in the wrong format.
            Atom count from _chemical_formula_sum:   C20 H28 O20 Sr2
            Atom count from _chemical_formula_moiety:C15 H23 O16 Sr2

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
  10 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

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

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Computing details

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.

Poly[[tetraaquatris(monomethyl fumarato)distrontium(II)] monomethyl fumarate] at 120 K

Crystal data

[Sr2(C5H5O4)3(H2O)4](C5H5O4)	Z = 2
Mr = 763.66	F(000) = 768
Triclinic, P1	Dx = 1.713 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.1336 (6) Å	Cell parameters from 5146 reflections
b = 10.7203 (8) Å	θ = 2.5–30.5°
c = 20.9384 (17) Å	µ = 3.69 mm^−1
α = 100.676 (2)°	T = 120 K
β = 96.322 (2)°	Needle, colorless
γ = 107.096 (2)°	0.23 × 0.05 × 0.03 mm
V = 1480.7 (2) Å^3

Data collection

Bruker SMART APEX diffractometer	8421 independent reflections
Radiation source: fine-focus sealed tube	5753 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.057
ω scan, frame data integration	θmax = 30.8°, θmin = 1.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	h = −10→10
Tmin = 0.484, Tmax = 0.897	k = −14→14
19750 measured reflections	l = −29→29

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)] = 0.038	Hydrogen site location: difference Fourier map
wR(F^2) = 0.095	H atoms treated by a mixture of independent and constrained refinement
S = 0.87	w = 1/[σ^2(Fo^2) + (0.0363P)^2] where P = (Fo^2 + 2Fc^2)/3
8421 reflections	(Δ/σ)max = 0.001
407 parameters	Δρmax = 1.48 e Å^−3
8 restraints	Δρmin = −0.71 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Sr1	0.37047 (4)	0.78079 (3)	0.464363 (15)	0.00913 (8)
Sr2	0.76100 (5)	0.60979 (3)	0.364673 (15)	0.01050 (8)
O1	0.9026 (4)	0.4145 (2)	0.38735 (12)	0.0150 (5)
H1A	0.925 (6)	0.385 (4)	0.3504 (12)	0.022*
H1B	0.825 (5)	0.344 (2)	0.3907 (19)	0.022*
O2	0.4592 (4)	0.4184 (2)	0.38307 (12)	0.0148 (5)
H2A	0.489 (6)	0.355 (3)	0.3917 (18)	0.022*
H2B	0.391 (5)	0.387 (3)	0.3452 (11)	0.022*
O3	0.2609 (4)	0.5330 (3)	0.47479 (13)	0.0169 (5)
H3A	0.149 (3)	0.500 (4)	0.4534 (17)	0.025*
H3B	0.327 (5)	0.502 (4)	0.4525 (17)	0.025*
O4	0.6638 (4)	0.4513 (3)	0.24953 (13)	0.0212 (6)
H4A	0.549 (3)	0.401 (3)	0.237 (2)	0.032*
H4B	0.739 (5)	0.409 (4)	0.243 (2)	0.032*
O11	0.7035 (3)	0.7471 (2)	0.47641 (12)	0.0153 (5)
O12	1.0237 (3)	0.7731 (2)	0.47988 (12)	0.0167 (5)
O13	1.1506 (4)	1.1838 (2)	0.68818 (12)	0.0179 (6)
O14	0.9678 (4)	0.9913 (2)	0.71089 (12)	0.0191 (6)
C11	0.8803 (5)	0.7869 (3)	0.50755 (17)	0.0122 (7)
C12	0.9135 (5)	0.8580 (3)	0.57931 (17)	0.0135 (7)
H12	0.8442	0.8137	0.6080	0.016*
C13	1.0387 (5)	0.9820 (3)	0.60273 (17)	0.0153 (7)
H13	1.1189	1.0209	0.5749	0.018*
C14	1.0590 (5)	1.0631 (4)	0.67101 (17)	0.0140 (7)
C15	0.9823 (6)	1.0658 (4)	0.77825 (18)	0.0242 (9)
H15A	0.9209	1.0050	0.8040	0.029*
H15B	0.9154	1.1314	0.7773	0.029*
H15C	1.1199	1.1101	0.7977	0.029*
O21	0.4119 (3)	0.7955 (2)	0.59156 (11)	0.0130 (5)
O22	0.5072 (4)	1.0017 (2)	0.57288 (12)	0.0153 (5)
O23	0.4712 (4)	1.0895 (3)	0.82092 (13)	0.0298 (7)
O24	0.4931 (4)	0.8917 (3)	0.83906 (12)	0.0220 (6)
C21	0.4659 (5)	0.9235 (3)	0.61189 (17)	0.0125 (7)
C22	0.4766 (5)	0.9847 (3)	0.68341 (16)	0.0139 (7)
H22	0.4936	1.0757	0.6961	0.017*
C23	0.4626 (5)	0.9124 (4)	0.72943 (17)	0.0162 (7)
H23	0.4445	0.8212	0.7172	0.019*
C24	0.4756 (5)	0.9765 (4)	0.80037 (17)	0.0163 (8)
C25	0.5151 (6)	0.9464 (4)	0.90965 (18)	0.0288 (10)
H25A	0.5269	0.8798	0.9334	0.035*
H25B	0.4005	0.9717	0.9184	0.035*
H25C	0.6325	1.0237	0.9236	0.035*
O31	0.4369 (3)	0.6700 (2)	0.34172 (11)	0.0140 (5)
O32	0.1293 (3)	0.6676 (2)	0.35228 (11)	0.0147 (5)
O33	0.0714 (4)	0.6071 (3)	0.10776 (13)	0.0316 (7)
O34	0.3740 (4)	0.6000 (3)	0.08954 (12)	0.0204 (6)
C31	0.2594 (5)	0.6540 (3)	0.31683 (17)	0.0116 (7)
C32	0.1965 (5)	0.6273 (3)	0.24360 (17)	0.0146 (7)
H32	0.0619	0.6083	0.2275	0.018*
C33	0.3189 (5)	0.6288 (3)	0.19956 (17)	0.0160 (7)
H33	0.4528	0.6409	0.2132	0.019*
C34	0.2388 (6)	0.6108 (4)	0.12808 (18)	0.0185 (8)
C35	0.3050 (6)	0.5881 (4)	0.01948 (18)	0.0287 (10)
H35A	0.4117	0.5863	−0.0045	0.034*
H35B	0.2628	0.6635	0.0144	0.034*
H35C	0.1952	0.5068	0.0026	0.034*
O41	0.7302 (4)	0.6780 (2)	0.74164 (12)	0.0205 (6)
O42	1.0410 (4)	0.6745 (3)	0.73507 (12)	0.0228 (6)
O43	1.0898 (4)	0.8464 (3)	0.98108 (13)	0.0334 (7)
O44	0.7678 (4)	0.7697 (3)	0.98973 (12)	0.0233 (6)
C41	0.9075 (6)	0.6944 (3)	0.76642 (18)	0.0174 (8)
C42	0.9677 (6)	0.7409 (4)	0.84034 (18)	0.0199 (8)
H42	1.1032	0.7698	0.8575	0.024*
C43	0.8443 (5)	0.7441 (4)	0.88308 (17)	0.0184 (8)
H43	0.7080	0.7154	0.8674	0.022*
C44	0.9180 (6)	0.7924 (4)	0.95524 (18)	0.0196 (8)
C45	0.8254 (6)	0.8163 (4)	1.06102 (18)	0.0270 (9)
H45A	0.7084	0.7990	1.0810	0.032*
H45B	0.8958	0.9108	1.0720	0.032*
H45C	0.9101	0.7697	1.0771	0.032*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sr1	0.00562 (16)	0.01074 (16)	0.01153 (16)	0.00271 (13)	0.00227 (12)	0.00316 (13)
Sr2	0.00568 (16)	0.01159 (16)	0.01408 (17)	0.00284 (13)	0.00240 (13)	0.00206 (13)
O1	0.0135 (13)	0.0142 (13)	0.0175 (13)	0.0027 (11)	0.0060 (11)	0.0052 (11)
O2	0.0132 (13)	0.0144 (13)	0.0182 (13)	0.0052 (11)	0.0020 (11)	0.0062 (11)
O3	0.0117 (13)	0.0164 (13)	0.0210 (15)	0.0034 (11)	0.0025 (11)	0.0027 (11)
O4	0.0188 (15)	0.0211 (15)	0.0202 (15)	0.0049 (12)	0.0021 (12)	−0.0007 (12)
O11	0.0074 (12)	0.0204 (13)	0.0168 (13)	0.0058 (11)	0.0007 (10)	−0.0003 (11)
O12	0.0104 (13)	0.0213 (13)	0.0175 (13)	0.0053 (11)	0.0054 (10)	0.0004 (11)
O13	0.0159 (14)	0.0152 (13)	0.0227 (14)	0.0040 (11)	0.0042 (11)	0.0055 (11)
O14	0.0213 (15)	0.0193 (13)	0.0166 (13)	0.0044 (11)	0.0083 (11)	0.0041 (11)
C11	0.0117 (18)	0.0077 (16)	0.0189 (18)	0.0038 (14)	0.0030 (14)	0.0058 (14)
C12	0.0084 (17)	0.0199 (18)	0.0145 (18)	0.0057 (15)	0.0036 (14)	0.0064 (15)
C13	0.0116 (18)	0.0205 (19)	0.0161 (18)	0.0057 (15)	0.0041 (14)	0.0078 (15)
C14	0.0103 (17)	0.0202 (19)	0.0145 (18)	0.0075 (15)	0.0021 (14)	0.0073 (15)
C15	0.026 (2)	0.029 (2)	0.017 (2)	0.0073 (18)	0.0057 (17)	0.0043 (17)
O21	0.0142 (13)	0.0117 (12)	0.0138 (12)	0.0048 (10)	0.0039 (10)	0.0030 (10)
O22	0.0158 (13)	0.0130 (12)	0.0174 (13)	0.0028 (10)	0.0038 (11)	0.0067 (10)
O23	0.047 (2)	0.0194 (15)	0.0225 (15)	0.0100 (14)	0.0127 (14)	0.0021 (12)
O24	0.0270 (16)	0.0303 (15)	0.0133 (13)	0.0140 (13)	0.0043 (11)	0.0079 (12)
C21	0.0061 (16)	0.0170 (18)	0.0169 (18)	0.0055 (14)	0.0041 (14)	0.0063 (15)
C22	0.0126 (18)	0.0132 (17)	0.0149 (18)	0.0038 (14)	0.0032 (14)	0.0010 (14)
C23	0.0150 (19)	0.0179 (18)	0.0151 (18)	0.0057 (15)	0.0018 (15)	0.0020 (15)
C24	0.0114 (18)	0.0214 (19)	0.0151 (18)	0.0024 (15)	0.0036 (14)	0.0055 (15)
C25	0.031 (2)	0.044 (3)	0.015 (2)	0.016 (2)	0.0041 (17)	0.0082 (19)
O31	0.0085 (12)	0.0184 (13)	0.0160 (13)	0.0062 (10)	0.0003 (10)	0.0044 (10)
O32	0.0099 (12)	0.0190 (13)	0.0141 (12)	0.0050 (11)	0.0025 (10)	0.0005 (10)
O33	0.0196 (16)	0.060 (2)	0.0185 (15)	0.0170 (15)	0.0019 (12)	0.0107 (14)
O34	0.0203 (14)	0.0312 (15)	0.0127 (13)	0.0113 (12)	0.0064 (11)	0.0052 (11)
C31	0.0108 (17)	0.0075 (16)	0.0174 (18)	0.0031 (14)	0.0037 (14)	0.0046 (14)
C32	0.0110 (18)	0.0132 (17)	0.0192 (19)	0.0043 (14)	−0.0002 (14)	0.0034 (15)
C33	0.0132 (18)	0.0181 (18)	0.0174 (19)	0.0060 (15)	0.0027 (15)	0.0045 (15)
C34	0.021 (2)	0.0196 (19)	0.0173 (19)	0.0072 (17)	0.0068 (16)	0.0063 (16)
C35	0.030 (2)	0.042 (3)	0.016 (2)	0.013 (2)	0.0060 (18)	0.0078 (19)
O41	0.0151 (14)	0.0255 (14)	0.0196 (14)	0.0063 (12)	0.0010 (11)	0.0036 (12)
O42	0.0196 (15)	0.0301 (15)	0.0197 (14)	0.0099 (12)	0.0081 (12)	0.0022 (12)
O43	0.0174 (16)	0.056 (2)	0.0187 (15)	0.0049 (15)	−0.0004 (12)	0.0020 (14)
O44	0.0187 (14)	0.0363 (16)	0.0160 (14)	0.0096 (13)	0.0066 (11)	0.0055 (12)
C41	0.019 (2)	0.0130 (18)	0.020 (2)	0.0040 (15)	0.0043 (16)	0.0035 (15)
C42	0.0131 (19)	0.023 (2)	0.021 (2)	0.0042 (16)	0.0021 (16)	0.0009 (16)
C43	0.0144 (19)	0.023 (2)	0.0182 (19)	0.0064 (16)	0.0029 (15)	0.0051 (16)
C44	0.023 (2)	0.023 (2)	0.0160 (19)	0.0120 (17)	0.0053 (16)	0.0040 (16)
C45	0.029 (2)	0.038 (2)	0.016 (2)	0.013 (2)	0.0070 (17)	0.0055 (18)

Geometric parameters (Å, º)

Sr1—O11	2.499 (2)	O22—C21	1.272 (4)
Sr1—O12^i	2.509 (2)	O23—C24	1.219 (4)
Sr1—O22^ii	2.537 (2)	O24—C24	1.348 (4)
Sr1—O3	2.598 (3)	O24—C25	1.458 (4)
Sr1—O32	2.601 (2)	C21—C22	1.503 (5)
Sr1—O21	2.617 (2)	C22—C23	1.338 (4)
Sr1—O31	2.775 (2)	C22—H22	0.9300
Sr1—O22	2.807 (2)	C23—C24	1.497 (5)
Sr2—O4	2.569 (3)	C23—H23	0.9300
Sr2—O32^iii	2.571 (2)	C25—H25A	0.9599
Sr2—O31	2.597 (2)	C25—H25B	0.9599
Sr2—O13^iv	2.600 (2)	C25—H25C	0.9599
Sr2—O2	2.621 (2)	O31—C31	1.264 (4)
Sr2—O11	2.664 (2)	O32—C31	1.275 (4)
Sr2—O1	2.671 (2)	O33—C34	1.209 (4)
Sr2—O12	2.812 (2)	O34—C34	1.341 (4)
O1—H1A	0.834 (18)	O34—C35	1.465 (4)
O1—H1B	0.818 (18)	C31—C32	1.498 (5)
O2—H2A	0.809 (18)	C32—C33	1.337 (5)
O2—H2B	0.837 (18)	C32—H32	0.9300
O3—H3A	0.810 (18)	C33—C34	1.498 (5)
O3—H3B	0.792 (18)	C33—H33	0.9300
O4—H4A	0.821 (19)	C35—H35A	0.9599
O4—H4B	0.807 (18)	C35—H35B	0.9599
O11—C11	1.264 (4)	C35—H35C	0.9599
O12—C11	1.262 (4)	O41—C41	1.261 (4)
O13—C14	1.229 (4)	O42—C41	1.261 (4)
O14—C14	1.333 (4)	O43—C44	1.204 (4)
O14—C15	1.463 (4)	O44—C44	1.346 (4)
C11—C12	1.512 (5)	O44—C45	1.454 (4)
C12—C13	1.330 (5)	C41—C42	1.507 (5)
C12—H12	0.9300	C42—C43	1.325 (5)
C13—C14	1.497 (5)	C42—H42	0.9300
C13—H13	0.9300	C43—C44	1.484 (5)
C15—H15A	0.9599	C43—H43	0.9300
C15—H15B	0.9599	C45—H45A	0.9599
C15—H15C	0.9599	C45—H45B	0.9599
O21—C21	1.284 (4)	C45—H45C	0.9599
H1A—O1—H1B	96 (4)	O23—C24—C23	125.3 (3)
H2A—O2—H2B	103 (4)	O24—C24—C23	110.6 (3)
H3A—O3—H3B	104 (4)	C34—O34—C35	114.2 (3)
H4A—O4—H4B	109 (4)	O31—C31—O32	122.2 (3)
C14—O14—C15	115.5 (3)	O31—C31—C32	120.9 (3)
O12—C11—O11	122.1 (3)	O32—C31—C32	116.8 (3)
O12—C11—C12	121.3 (3)	C33—C32—C31	125.0 (3)
O11—C11—C12	116.6 (3)	C32—C33—C34	119.5 (3)
C13—C12—C11	122.1 (3)	O33—C34—O34	124.1 (3)
C12—C13—C14	124.3 (3)	O33—C34—C33	123.6 (3)
O13—C14—O14	123.7 (3)	O34—C34—C33	112.3 (3)
O13—C14—C13	123.0 (3)	C44—O44—C45	115.6 (3)
O14—C14—C13	113.3 (3)	O42—C41—O41	126.1 (3)
C24—O24—C25	115.0 (3)	O42—C41—C42	116.1 (3)
O22—C21—O21	122.0 (3)	O41—C41—C42	117.9 (3)
O22—C21—C22	118.1 (3)	C43—C42—C41	125.7 (4)
O21—C21—C22	119.9 (3)	C42—C43—C44	121.8 (4)
C23—C22—C21	122.1 (3)	O43—C44—O44	122.9 (3)
C22—C23—C24	120.9 (3)	O43—C44—C43	125.4 (3)
O23—C24—O24	124.1 (3)	O44—C44—C43	111.7 (3)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···O42^v	0.83 (2)	1.85 (2)	2.681 (3)	174 (4)
O1—H1B···O21^vi	0.82 (2)	2.02 (2)	2.813 (3)	163 (4)
O2—H2A···O21^vi	0.809 (18)	2.017 (19)	2.822 (3)	174 (4)
O2—H2B···O41^vi	0.837 (18)	1.835 (19)	2.667 (3)	173 (4)
O3—H3A···O1^i	0.810 (18)	1.98 (2)	2.775 (4)	169 (4)
O3—H3B···O2	0.792 (18)	2.03 (2)	2.819 (4)	171 (4)
O4—H4A···O41^vi	0.821 (19)	2.05 (3)	2.788 (4)	149 (4)
O4—H4B···O42^v	0.807 (18)	2.07 (2)	2.835 (4)	159 (4)

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