Poly[di-μ₃-aqua-μ₄-terephthalato-dicaesium]

Colourless platelets of dicaesium terephthalate dihydrate, [Cs₂(C₈O₄H₄)(H₂O)₂]_n, were obtained from an aqueous solution of Cs₂CO₃, NaOH and terephthalic acid in demineral­ized water and subsequent evaporation of the solvent at room temperature. Caesium is coordinated by four O atoms from four water mol­ecules and four O atoms from four different centrosymmetric terephthalates. The metal centres are connected by the water mol­ecules, forming a double layer parallel to (011). These double layers are linked by the terephthalate dianions, forming a three-dimensional framework structure.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.033
• wR factor = 0.082
• Data-to-parameter ratio = 17.0

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor       O3     -   H1     ...          ?
PLAT420_ALERT_2_B D-H Without Acceptor       O3     -   H2     ...          ?

Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.96
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.23 Ratio
PLAT731_ALERT_1_C Bond    Calc     0.96(7), Rep     0.96(2) ......       3.50 su-Ra
              O3   -H1      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.96(8), Rep     0.96(2) ......       4.00 su-Ra
              O3   -H2      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.96(7), Rep     0.96(2) ......       3.50 su-Ra
              O3   -H1      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.96(8), Rep     0.96(2) ......       4.00 su-Ra
              O3   -H2      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.96(8), Rep     0.96(2) ......       4.00 su-Ra
              O3   -H2      1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     1.86(8), Rep     1.85(3) ......       2.67 su-Ra
              H1   -O2      1.555   2.645
PLAT736_ALERT_1_C H...A   Calc     2.42(9), Rep     2.42(4) ......       2.25 su-Ra
              H2   -O1      1.555   2.655
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.21 Ratio

Alert level G
ABSTM02_ALERT_3_G  The ratio of expected to reported Tmax/Tmin(RR) is > 2.00
            Tmin and Tmax reported:      0.270     0.637
            Tmin and Tmax expected:      0.130     0.658
            RR =      2.148
            Please check that your absorption correction is appropriate.

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

   8 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
   3 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-RED (Stoe & Cie, 2001); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97.

Poly[di-µ₃-aqua-µ₄-terephthalato-dicaesium]

Crystal data

[Cs2(C8H4O4)(H2O)2]	F(000) = 428
Mr = 232.98	Dx = 2.535 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 1491 reflections
a = 12.729 (4) Å	θ = 3.0–28.1°
b = 4.1724 (7) Å	µ = 5.98 mm^−1
c = 12.498 (4) Å	T = 295 K
β = 113.10 (3)°	Plate, colourless
V = 610.6 (3) Å^3	0.4 × 0.3 × 0.07 mm
Z = 4

Data collection

Stoe IPDS-I diffractometer	1431 independent reflections
Radiation source: fine-focus sealed tube	1088 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.088
φ scans	θmax = 28.0°, θmin = 3.3°
Absorption correction: numerical (X-RED; Stoe & Cie, 2001); crystal shape optimized by X-SHAPE (Stoe & Cie, 1999)	h = −16→16
Tmin = 0.270, Tmax = 0.637	k = −5→5
6555 measured reflections	l = −16→16

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.033	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.082	w = 1/[σ^2(Fo^2) + (0.0457P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.96	(Δ/σ)max < 0.001
1431 reflections	Δρmax = 0.82 e Å^−3
84 parameters	Δρmin = −1.38 e Å^−3
2 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.013 (1)

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
Cs1	0.65809 (3)	0.28904 (8)	0.18665 (3)	0.03645 (18)
O1	0.7620 (4)	0.7105 (11)	0.5820 (4)	0.0471 (11)
O2	0.7060 (3)	0.8080 (10)	0.3922 (4)	0.0415 (10)
O3	0.4483 (3)	0.7666 (11)	0.0997 (4)	0.0430 (10)
C1	0.7794 (4)	0.7193 (12)	0.4908 (4)	0.0260 (10)
C2	0.8939 (4)	0.6101 (12)	0.4958 (4)	0.0252 (10)
C3	0.9687 (4)	0.4512 (13)	0.5931 (4)	0.0300 (11)
H3	0.9480	0.4152	0.6556	0.031 (14)*
C4	0.9259 (4)	0.6551 (14)	0.4010 (4)	0.0307 (11)
H4	0.8761	0.7566	0.3340	0.05 (2)*
H1	0.390 (6)	0.607 (17)	0.083 (7)	0.08 (3)*
H2	0.384 (6)	0.91 (2)	0.070 (8)	0.10 (3)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cs1	0.0409 (2)	0.0352 (3)	0.0373 (2)	0.00108 (16)	0.01964 (15)	0.00273 (14)
O1	0.042 (2)	0.058 (3)	0.055 (3)	0.0177 (19)	0.034 (2)	0.0131 (19)
O2	0.0263 (18)	0.052 (3)	0.043 (2)	0.0125 (17)	0.0101 (17)	−0.0001 (18)
O3	0.0257 (19)	0.048 (3)	0.055 (2)	−0.0010 (17)	0.0149 (18)	0.0045 (19)
C1	0.023 (2)	0.025 (3)	0.035 (2)	0.0000 (18)	0.0166 (19)	−0.0024 (19)
C2	0.021 (2)	0.022 (3)	0.033 (2)	−0.0012 (18)	0.012 (2)	−0.0019 (18)
C3	0.026 (3)	0.041 (3)	0.028 (2)	0.003 (2)	0.015 (2)	0.004 (2)
C4	0.022 (2)	0.041 (3)	0.027 (2)	0.005 (2)	0.0077 (19)	0.008 (2)

Geometric parameters (Å, º)

Cs1—O1^i	3.027 (4)	O1—C1	1.244 (6)
Cs1—O1^ii	3.030 (4)	O2—C1	1.275 (7)
Cs1—O2^iii	3.125 (4)	O3—H1	0.96 (2)
Cs1—O3	3.163 (4)	O3—H2	0.96 (2)
Cs1—O2	3.229 (4)	C1—C2	1.505 (6)
Cs1—O3^iii	3.285 (4)	C2—C3	1.385 (7)
Cs1—O3^iv	3.301 (5)	C2—C4	1.408 (7)
Cs1—O3^v	3.436 (5)	C3—C4^vii	1.387 (7)
Cs1—Cs1^iii	4.1724 (7)	C3—H3	0.9300
Cs1—Cs1^vi	4.1724 (7)	C4—H4	0.9300
Cs1—Cs1^iv	5.131 (2)
O1^i—Cs1—O1^ii	87.09 (10)	O2^iii—Cs1—Cs1^iv	142.95 (8)
O1^i—Cs1—O2^iii	86.30 (12)	O3—Cs1—Cs1^iv	38.40 (9)
O1^ii—Cs1—O2^iii	145.08 (12)	O2—Cs1—Cs1^iv	109.22 (7)
O1^i—Cs1—O3	137.60 (13)	O3^iii—Cs1—Cs1^iv	71.40 (8)
O1^ii—Cs1—O3	82.55 (12)	O3^iv—Cs1—Cs1^iv	36.53 (8)
O2^iii—Cs1—O3	123.58 (11)	O3^v—Cs1—Cs1^iv	107.95 (8)
O1^i—Cs1—O2	145.81 (11)	C4—Cs1—Cs1^iv	132.92 (9)
O1^ii—Cs1—O2	84.43 (11)	Cs1^iii—Cs1—Cs1^iv	110.065 (12)
O2^iii—Cs1—O2	82.06 (10)	Cs1^vi—Cs1—Cs1^iv	69.935 (12)
O3—Cs1—O2	73.82 (11)	O1^i—Cs1—H1	130.3 (12)
O1^i—Cs1—O3^iii	80.59 (11)	O1^ii—Cs1—H1	96.3 (9)
O1^ii—Cs1—O3^iii	138.65 (12)	O2^iii—Cs1—H1	113.9 (11)
O2^iii—Cs1—O3^iii	73.55 (11)	O3—Cs1—H1	16.2 (7)
O3—Cs1—O3^iii	80.62 (10)	O2—Cs1—H1	83.6 (11)
O2—Cs1—O3^iii	125.70 (11)	O3^iii—Cs1—H1	64.5 (7)
O1^i—Cs1—O3^iv	62.99 (12)	O3^iv—Cs1—H1	72.1 (13)
O1^ii—Cs1—O3^iv	69.09 (11)	O3^v—Cs1—H1	70.3 (13)
O2^iii—Cs1—O3^iv	135.30 (11)	C4—Cs1—H1	127.5 (10)
O3—Cs1—O3^iv	74.93 (13)	Cs1^iii—Cs1—H1	112.9 (7)
O2—Cs1—O3^iv	141.14 (11)	Cs1^vi—Cs1—H1	67.1 (7)
O3^iii—Cs1—O3^iv	70.14 (13)	Cs1^iv—Cs1—H1	37.9 (13)
O1^i—Cs1—O3^v	133.57 (11)	C1—O1—Cs1^viii	133.0 (4)
O1^ii—Cs1—O3^v	136.56 (11)	C1—O1—Cs1^ix	129.8 (3)
O2^iii—Cs1—O3^v	49.71 (10)	Cs1^viii—O1—Cs1^ix	87.09 (10)
O3—Cs1—O3^v	75.35 (12)	C1—O2—Cs1^vi	144.5 (3)
O2—Cs1—O3^v	53.80 (11)	C1—O2—Cs1	114.4 (3)
O3^iii—Cs1—O3^v	73.84 (12)	Cs1^vi—O2—Cs1	82.06 (10)
O3^iv—Cs1—O3^v	136.19 (13)	Cs1—O3—Cs1^vi	80.62 (10)
O1^i—Cs1—C4	99.26 (12)	Cs1—O3—Cs1^iv	105.07 (13)
O1^ii—Cs1—C4	66.29 (12)	Cs1^vi—O3—Cs1^iv	109.86 (13)
O2^iii—Cs1—C4	81.04 (11)	Cs1—O3—Cs1^x	106.70 (13)
O3—Cs1—C4	113.49 (12)	Cs1^vi—O3—Cs1^x	104.01 (13)
O2—Cs1—C4	47.25 (11)	Cs1^iv—O3—Cs1^x	136.51 (13)
O3^iii—Cs1—C4	154.56 (11)	Cs1—O3—H1	97 (6)
O3^iv—Cs1—C4	132.59 (11)	Cs1^vi—O3—H1	174 (5)
O3^v—Cs1—C4	88.90 (11)	Cs1^iv—O3—H1	76 (5)
O1^i—Cs1—Cs1^iii	46.48 (8)	Cs1^x—O3—H1	71 (5)
O1^ii—Cs1—Cs1^iii	133.57 (8)	Cs1—O3—H2	177 (6)
O2^iii—Cs1—Cs1^iii	50.05 (8)	Cs1^vi—O3—H2	100 (7)
O3—Cs1—Cs1^iii	129.04 (8)	Cs1^iv—O3—H2	72 (6)
O2—Cs1—Cs1^iii	132.11 (8)	Cs1^x—O3—H2	76 (6)
O3^iii—Cs1—Cs1^iii	48.42 (8)	H1—O3—H2	83 (9)
O3^iv—Cs1—Cs1^iii	85.97 (8)	O1—C1—O2	124.7 (5)
O3^v—Cs1—Cs1^iii	88.44 (7)	O1—C1—C2	118.1 (4)
C4—Cs1—Cs1^iii	114.13 (8)	O2—C1—C2	117.2 (4)
O1^i—Cs1—Cs1^vi	133.52 (8)	C3—C2—C4	118.4 (4)
O1^ii—Cs1—Cs1^vi	46.43 (8)	C3—C2—C1	120.2 (4)
O2^iii—Cs1—Cs1^vi	129.95 (8)	C4—C2—C1	121.3 (4)
O3—Cs1—Cs1^vi	50.96 (8)	C2—C3—C4^vii	121.2 (4)
O2—Cs1—Cs1^vi	47.89 (8)	C2—C3—H3	119.4
O3^iii—Cs1—Cs1^vi	131.58 (8)	C4^vii—C3—H3	119.4
O3^iv—Cs1—Cs1^vi	94.03 (8)	C3^vii—C4—C2	120.4 (4)
O3^v—Cs1—Cs1^vi	91.56 (7)	C3^vii—C4—Cs1	119.9 (4)
C4—Cs1—Cs1^vi	65.87 (8)	C2—C4—Cs1	93.7 (3)
Cs1^iii—Cs1—Cs1^vi	180.000 (11)	C3^vii—C4—H4	119.8
O1^i—Cs1—Cs1^iv	99.38 (9)	C2—C4—H4	119.8
O1^ii—Cs1—Cs1^iv	71.97 (9)	Cs1—C4—H4	55.5

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H1···O2^v	0.96 (2)	1.85 (3)	2.772 (6)	160 (7)
O3—H2···O2^x	0.96 (2)	2.18 (6)	3.021 (6)	146 (8)
O3—H2···O1^x	0.96 (2)	2.42 (4)	3.314 (7)	155 (8)

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