catena-Poly­[[di­aqua­calcium(II)]-μ₃-terephthalato-μ₂-aqua] at 150 K

The title compound, [Ca(C₈H₄O₄)(H₂O)₃]_n, has been previously studied by single-crystal X-ray diffraction at both room temperature [Matsuzaki & Iitaka (1972). Acta Cryst. B28, 1977–1981] and 173 K [Groeneman & Atwood (1999). Cryst. Eng. 2, 241–249.]. We present here a redetermination of the compound at 150 K, which results in a considerably improved precision and the location of H atoms in the strong O—H...O hydrogen bonds.

Key indicators

• Single-crystal X-ray study
• T = 150 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.054
• wR factor = 0.143
• Data-to-parameter ratio = 14.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



REFLT_03
         From the CIF: _diffrn_reflns_theta_max           28.66
         From the CIF: _reflns_number_total               2362
         TEST2: Reflns within _diffrn_reflns_theta_max
         Count of symmetry unique reflns         2577
         Completeness (_total/calc)             91.66%
          Alert C: < 95% complete


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 1 Alert Level C = Please check

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Computing details

Data collection: SMART (Siemens, 1994); cell refinement: SAINT (Siemens, 1994); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and local programs.

(I)

Crystal data

[Ca(C8H4O4)(H2O)3]	F(000) = 536
Mr = 258.24	Dx = 1.718 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2161 reflections
a = 7.0455 (15) Å	θ = 2.9–27.9°
b = 21.623 (4) Å	µ = 0.65 mm^−1
c = 6.5622 (13) Å	T = 150 K
β = 92.831 (3)°	Column, colourless
V = 998.5 (3) Å^3	0.78 × 0.06 × 0.05 mm
Z = 4

Data collection

Bruker SMART 1000 CCD diffractometer	2362 independent reflections
Radiation source: sealed tube	1751 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.055
ω rotation with narrow frames scans	θmax = 28.7°, θmin = 1.9°
Absorption correction: multi-scan (Sheldrick, 2001)	h = −8→9
Tmin = 0.632, Tmax = 0.968	k = −29→28
8282 measured reflections	l = −8→8

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: All non-H atoms found by direct methods
R[F^2 > 2σ(F^2)] = 0.054	Hydrogen site location: Geom except OH coords freely refined
wR(F^2) = 0.143	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0811P)^2 + 0.4161P] where P = (Fo^2 + 2Fc^2)/3
2362 reflections	(Δ/σ)max = 0.001
163 parameters	Δρmax = 1.40 e Å^−3
18 restraints	Δρmin = −0.48 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.16484 (9)	0.78543 (3)	0.49411 (9)	0.01134 (19)
C1	0.2503 (4)	0.91382 (14)	0.9929 (5)	0.0116 (6)
C2	0.2836 (4)	0.94604 (14)	0.8147 (5)	0.0138 (6)
H2	0.3024	0.9242	0.6918	0.017*
C3	0.2892 (5)	1.01023 (14)	0.8167 (4)	0.0139 (6)
H3	0.3121	1.0321	0.6946	0.017*
C4	0.2618 (4)	1.04294 (14)	0.9955 (5)	0.0118 (6)
C5	0.2282 (5)	1.01007 (14)	1.1734 (5)	0.0157 (7)
H5	0.2087	1.0317	1.2966	0.019*
C6	0.2233 (5)	0.94600 (14)	1.1712 (5)	0.0153 (7)
H6	0.2012	0.9240	1.2931	0.018*
C7	0.2407 (4)	0.84443 (14)	0.9926 (4)	0.0107 (6)
O1	0.2214 (3)	0.81659 (10)	1.1583 (3)	0.0148 (5)
O2	0.2519 (3)	0.81539 (10)	0.8282 (3)	0.0136 (5)
C8	0.2676 (4)	1.11249 (14)	0.9989 (4)	0.0113 (6)
O3	0.2782 (3)	1.14050 (10)	0.8317 (3)	0.0154 (5)
O4	0.2585 (3)	1.13924 (10)	1.1682 (3)	0.0154 (5)
O5	−0.0931 (3)	0.74923 (10)	0.2476 (4)	0.0155 (5)
H5A	−0.151 (5)	0.7188 (12)	0.273 (6)	0.023*
H5B	−0.151 (5)	0.7787 (13)	0.207 (6)	0.023*
O6	−0.0340 (3)	0.87359 (10)	0.5026 (3)	0.0166 (5)
H6A	−0.085 (5)	0.8762 (19)	0.609 (4)	0.025*
H6B	−0.103 (5)	0.8722 (19)	0.401 (4)	0.025*
O7	0.4810 (4)	0.82427 (14)	0.4946 (4)	0.0288 (6)
H7A	0.538 (6)	0.832 (2)	0.601 (4)	0.043*
H7B	0.528 (6)	0.837 (2)	0.394 (4)	0.043*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0156 (3)	0.0103 (3)	0.0083 (3)	0.0005 (2)	0.0017 (2)	0.0001 (2)
C1	0.0108 (14)	0.0132 (15)	0.0109 (15)	−0.0004 (11)	0.0002 (11)	0.0002 (11)
C2	0.0178 (16)	0.0117 (15)	0.0118 (15)	0.0009 (12)	0.0021 (12)	−0.0042 (11)
C3	0.0194 (17)	0.0135 (15)	0.0089 (15)	−0.0003 (12)	0.0021 (12)	0.0034 (11)
C4	0.0118 (14)	0.0112 (14)	0.0124 (15)	0.0002 (11)	0.0011 (11)	−0.0003 (11)
C5	0.0243 (18)	0.0121 (15)	0.0110 (15)	−0.0016 (12)	0.0036 (13)	−0.0004 (11)
C6	0.0224 (17)	0.0142 (15)	0.0096 (15)	0.0001 (12)	0.0036 (13)	0.0019 (11)
C7	0.0108 (14)	0.0131 (14)	0.0083 (14)	0.0007 (11)	0.0004 (10)	−0.0018 (11)
O1	0.0210 (12)	0.0134 (11)	0.0103 (11)	−0.0017 (9)	0.0040 (9)	0.0019 (8)
O2	0.0202 (12)	0.0140 (11)	0.0068 (10)	−0.0024 (8)	0.0022 (8)	−0.0004 (8)
C8	0.0107 (14)	0.0128 (15)	0.0106 (14)	0.0002 (11)	0.0025 (11)	0.0019 (11)
O3	0.0222 (12)	0.0116 (10)	0.0125 (11)	0.0001 (9)	0.0014 (9)	0.0013 (8)
O4	0.0229 (12)	0.0132 (11)	0.0103 (11)	0.0007 (9)	0.0032 (9)	−0.0015 (8)
O5	0.0171 (11)	0.0111 (11)	0.0183 (12)	−0.0004 (8)	0.0006 (9)	0.0023 (9)
O6	0.0214 (12)	0.0195 (12)	0.0091 (11)	0.0009 (9)	0.0026 (9)	−0.0001 (9)
O7	0.0228 (14)	0.0513 (17)	0.0125 (12)	−0.0114 (12)	0.0020 (10)	−0.0022 (12)

Geometric parameters (Å, º)

Ca1—O2	2.339 (2)	C4—C5	1.397 (4)
Ca1—O1^i	2.357 (2)	C4—C8	1.504 (4)
Ca1—O6	2.368 (2)	C5—C6	1.386 (4)
Ca1—O7	2.380 (3)	C5—H5	0.9500
Ca1—O1^ii	2.479 (2)	C6—H6	0.9500
Ca1—O5	2.498 (2)	C7—O2	1.254 (3)
Ca1—O2^ii	2.526 (2)	C7—O1	1.256 (3)
Ca1—O5^iii	2.633 (2)	C8—O4	1.257 (3)
C1—C6	1.382 (4)	C8—O3	1.259 (3)
C1—C2	1.391 (4)	O5—H5A	0.80 (2)
C1—C7	1.502 (4)	O5—H5B	0.80 (2)
C2—C3	1.389 (4)	O6—H6A	0.80 (2)
C2—H2	0.9500	O6—H6B	0.81 (2)
C3—C4	1.392 (4)	O7—H7A	0.80 (2)
C3—H3	0.9500	O7—H7B	0.81 (2)
O2—Ca1—O1^i	138.47 (8)	C2—C3—H3	119.6
O2—Ca1—O6	83.29 (8)	C4—C3—H3	119.6
O1^i—Ca1—O6	85.37 (8)	C3—C4—C5	118.8 (3)
O2—Ca1—O7	72.48 (8)	C3—C4—C8	121.0 (3)
O1^i—Ca1—O7	72.48 (9)	C5—C4—C8	120.1 (3)
O6—Ca1—O7	105.70 (10)	C6—C5—C4	120.3 (3)
O2—Ca1—O1^ii	79.04 (7)	C6—C5—H5	119.8
O1^i—Ca1—O1^ii	129.04 (7)	C4—C5—H5	119.8
O6—Ca1—O1^ii	142.08 (8)	C1—C6—C5	120.5 (3)
O7—Ca1—O1^ii	100.54 (9)	C1—C6—H6	119.7
O2—Ca1—O5	147.40 (8)	C5—C6—H6	119.7
O1^i—Ca1—O5	68.63 (8)	O2—C7—O1	121.2 (3)
O6—Ca1—O5	81.67 (8)	O2—C7—C1	119.8 (3)
O7—Ca1—O5	139.66 (8)	O1—C7—C1	119.0 (3)
O1^ii—Ca1—O5	95.67 (8)	C7—O1—Ca1^iv	167.7 (2)
O2—Ca1—O2^ii	125.80 (8)	C7—O1—Ca1^iii	94.13 (17)
O1^i—Ca1—O2^ii	77.75 (7)	Ca1^iv—O1—Ca1^iii	96.95 (8)
O6—Ca1—O2^ii	149.48 (8)	C7—O2—Ca1	157.0 (2)
O7—Ca1—O2^ii	93.32 (9)	C7—O2—Ca1^iii	91.98 (17)
O1^ii—Ca1—O2^ii	51.83 (7)	Ca1—O2—Ca1^iii	96.14 (8)
O5—Ca1—O2^ii	68.59 (8)	O4—C8—O3	123.8 (3)
O2—Ca1—O5^iii	69.13 (8)	O4—C8—C4	118.1 (3)
O1^i—Ca1—O5^iii	145.70 (8)	O3—C8—C4	118.1 (3)
O6—Ca1—O5^iii	77.68 (8)	Ca1—O5—Ca1^ii	89.74 (8)
O7—Ca1—O5^iii	140.78 (8)	Ca1—O5—H5A	119 (3)
O1^ii—Ca1—O5^iii	64.73 (7)	Ca1^ii—O5—H5A	106 (3)
O5—Ca1—O5^iii	79.46 (7)	Ca1—O5—H5B	108 (3)
O2^ii—Ca1—O5^iii	102.51 (7)	Ca1^ii—O5—H5B	112 (3)
C6—C1—C2	119.7 (3)	H5A—O5—H5B	118 (3)
C6—C1—C7	119.7 (3)	Ca1—O6—H6A	112 (3)
C2—C1—C7	120.6 (3)	Ca1—O6—H6B	106 (3)
C3—C2—C1	119.9 (3)	H6A—O6—H6B	116 (3)
C3—C2—H2	120.0	Ca1—O7—H7A	120 (3)
C1—C2—H2	120.0	Ca1—O7—H7B	123 (3)
C2—C3—C4	120.7 (3)	H7A—O7—H7B	116 (3)
C6—C1—C2—C3	−0.1 (5)	O7—Ca1—O2—C7	122.0 (5)
C7—C1—C2—C3	179.0 (3)	O1^ii—Ca1—O2—C7	−133.1 (5)
C1—C2—C3—C4	0.0 (5)	O5—Ca1—O2—C7	−49.8 (6)
C2—C3—C4—C5	0.0 (5)	O2^ii—Ca1—O2—C7	−156.8 (5)
C2—C3—C4—C8	−180.0 (3)	O5^iii—Ca1—O2—C7	−66.2 (5)
C3—C4—C5—C6	0.3 (5)	O1^i—Ca1—O2—Ca1^iii	−161.60 (9)
C8—C4—C5—C6	−179.8 (3)	O6—Ca1—O2—Ca1^iii	123.19 (8)
C2—C1—C6—C5	0.3 (5)	O7—Ca1—O2—Ca1^iii	−127.97 (11)
C7—C1—C6—C5	−178.8 (3)	O1^ii—Ca1—O2—Ca1^iii	−23.10 (8)
C4—C5—C6—C1	−0.4 (5)	O5—Ca1—O2—Ca1^iii	60.24 (16)
C6—C1—C7—O2	175.0 (3)	O2^ii—Ca1—O2—Ca1^iii	−46.77 (15)
C2—C1—C7—O2	−4.1 (4)	O5^iii—Ca1—O2—Ca1^iii	43.86 (7)
C6—C1—C7—O1	−4.9 (4)	C3—C4—C8—O4	−173.9 (3)
C2—C1—C7—O1	175.9 (3)	C5—C4—C8—O4	6.2 (4)
O2—C7—O1—Ca1^iv	−163.1 (8)	C3—C4—C8—O3	7.3 (4)
C1—C7—O1—Ca1^iv	16.8 (11)	C5—C4—C8—O3	−172.7 (3)
O2—C7—O1—Ca1^iii	−9.3 (3)	O2—Ca1—O5—Ca1^ii	−163.92 (12)
C1—C7—O1—Ca1^iii	170.6 (2)	O1^i—Ca1—O5—Ca1^ii	44.43 (7)
O1—C7—O2—Ca1	119.9 (5)	O6—Ca1—O5—Ca1^ii	132.70 (8)
C1—C7—O2—Ca1	−60.0 (6)	O7—Ca1—O5—Ca1^ii	28.21 (16)
O1—C7—O2—Ca1^iii	9.1 (3)	O1^ii—Ca1—O5—Ca1^ii	−85.43 (7)
C1—C7—O2—Ca1^iii	−170.8 (2)	O2^ii—Ca1—O5—Ca1^ii	−40.34 (6)
O1^i—Ca1—O2—C7	88.4 (5)	O5^iii—Ca1—O5—Ca1^ii	−148.38 (10)
O6—Ca1—O2—C7	13.2 (5)

Symmetry codes: (i) x, y, z−1; (ii) x, −y+3/2, z−1/2; (iii) x, −y+3/2, z+1/2; (iv) x, y, z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5A···O4^v	0.80 (2)	1.93 (2)	2.717 (3)	172 (4)
O5—H5B···O3^vi	0.80 (2)	1.97 (2)	2.755 (3)	167 (4)
O6—H6B···O3^vi	0.81 (2)	1.93 (2)	2.737 (3)	173 (4)
O6—H6A···O4^vii	0.80 (2)	1.98 (2)	2.754 (3)	162 (4)
O7—H7A···O4^viii	0.80 (2)	2.13 (2)	2.914 (3)	165 (4)
O7—H7B···O3^ix	0.81 (2)	2.12 (3)	2.898 (3)	164 (4)

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