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

Colourless platelets of dirubidium terephthalate dihydrate, [Rb₂(C₈O₄H₄)(H₂O)₂]_n, were obtained by hydro­thermal reaction of Rb₂CO₃ and terephthalic acid in demineralized water followed by slow evaporation of the solvent at room temperature. Rubidium is coordinated by four O atoms from four water mol­ecules and four O atoms from four different centrosymmetric terephthalates. The metal centers are connected by the water mol­ecules, forming a double layer perpendicular to [100]. 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) = 0.007 Å
• R factor = 0.042
• wR factor = 0.103
• Data-to-parameter ratio = 14.8

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......       0.93

Alert level C
REFLT03_ALERT_3_C  Reflection count < 95% complete
           From the CIF: _diffrn_reflns_theta_max           28.04
           From the CIF: _diffrn_reflns_theta_full          28.04
           From the CIF: _reflns_number_total               1243
           TEST2: Reflns within _diffrn_reflns_theta_max
           Count of symmetry unique reflns         1332
           Completeness (_total/calc)             93.32%
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       2.00 Ratio
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          8
PLAT731_ALERT_1_C Bond    Calc  3.9531(12), Rep   3.9531(5) ......       2.40 su-Ra
              RB1  -RB1     1.555   1.565
PLAT731_ALERT_1_C Bond    Calc  3.9531(12), Rep   3.9531(5) ......       2.40 su-Ra
              RB1  -RB1     1.555   1.545
PLAT731_ALERT_1_C Bond    Calc     0.94(5), Rep     0.94(2) ......       2.50 su-Ra
              O3   -H1      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.95(5), Rep     0.94(2) ......       2.50 su-Ra
              O3   -H2      1.555   1.555
PLAT732_ALERT_1_C Angle   Calc     17.2(9), Rep     17.2(4) ......       2.25 su-Ra
              O3   -RB1  -H2      1.555   1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.94(5), Rep     0.94(2) ......       2.50 su-Ra
              O3   -H1      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.95(5), Rep     0.94(2) ......       2.50 su-Ra
              O3   -H2      1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.95(5), Rep     0.94(2) ......       2.50 su-Ra
              O3   -H2      1.555   1.555
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.23 Ratio

Alert level G
ABSTM02_ALERT_3_G  The ratio of expected to reported Tmax/Tmin(RR) is > 2.00
            Tmin and Tmax reported:      0.248     0.333
            Tmin and Tmax expected:      0.053     0.537
            RR =      7.545
            Please check that your absorption correction is appropriate.

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

  11 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 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-AREA; 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-dirubidium]

Crystal data

[Rb2(C8H4O4)(H2O)2]	F(000) = 356
Mr = 371.08	Dx = 2.234 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 1243 reflections
a = 12.663 (3) Å	θ = 3.0–28.0°
b = 3.9531 (5) Å	µ = 8.88 mm^−1
c = 11.873 (3) Å	T = 295 K
β = 111.87 (3)°	Plate, colorless
V = 551.6 (2) Å^3	0.4 × 0.3 × 0.07 mm
Z = 2

Data collection

Stoe IPDS IP diffractometer	1243 independent reflections
Radiation source: fine-focus sealed tube	874 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.091
φ scans	θmax = 28.0°, θmin = 3.5°
Absorption correction: numerical [X-RED32 (Stoe & Cie, 2001); crystal shape optimized by X-SHAPE (Stoe & Cie, 1999)]	h = −16→16
Tmin = 0.248, Tmax = 0.333	k = −4→4
5609 measured reflections	l = −15→15

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.042	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.103	w = 1/[σ^2(Fo^2) + (0.0625P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.96	(Δ/σ)max = 0.001
1243 reflections	Δρmax = 0.87 e Å^−3
84 parameters	Δρmin = −1.48 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: 0.015 (3)

Special details

Experimental. A suitable single-crystal was carefully selected under a polarizing microscope and mounted in a glass capillary. The scattering intensities were collected on an imaging plate diffractometer (IPDS I, Stoe & Cie) equipped with a fine focus sealed tube X-ray source (Mo Kα, λ = 0.71073 Å) operating at 50 kV and 40 mA.

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
Rb1	0.65483 (4)	0.79622 (13)	0.18263 (4)	0.0335 (2)
O2	0.7052 (3)	0.3109 (10)	0.3821 (3)	0.0335 (8)
O1	0.7521 (3)	0.2016 (11)	0.5772 (3)	0.0369 (9)
O3	0.4564 (3)	0.2658 (11)	0.1041 (4)	0.0393 (9)
C1	0.7751 (4)	0.2159 (12)	0.4845 (4)	0.0229 (9)
C2	0.8917 (4)	0.1065 (12)	0.4916 (4)	0.0203 (9)
C3	0.9264 (4)	0.1514 (13)	0.3939 (4)	0.0255 (10)
H3	0.8775	0.2528	0.3230	0.029 (14)*
C4	0.9664 (4)	−0.0449 (14)	0.5975 (4)	0.0253 (10)
H4	0.9442	−0.0748	0.6632	0.036 (16)*
H1	0.402 (4)	0.095 (12)	0.095 (5)	0.039 (16)*
H2	0.409 (5)	0.459 (12)	0.085 (6)	0.06 (2)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Rb1	0.0357 (3)	0.0330 (4)	0.0353 (3)	0.0016 (2)	0.0173 (2)	0.0030 (2)
O2	0.0191 (17)	0.046 (3)	0.0331 (18)	0.0095 (16)	0.0066 (14)	0.0025 (16)
O1	0.030 (2)	0.048 (3)	0.040 (2)	0.0107 (17)	0.0218 (17)	0.0073 (17)
O3	0.0229 (19)	0.037 (3)	0.058 (2)	0.0010 (16)	0.0147 (18)	0.0020 (18)
C1	0.022 (2)	0.020 (3)	0.029 (2)	−0.0019 (18)	0.0127 (19)	−0.0024 (18)
C2	0.017 (2)	0.022 (3)	0.024 (2)	−0.0018 (16)	0.0100 (18)	−0.0009 (17)
C3	0.020 (2)	0.035 (3)	0.019 (2)	0.0062 (19)	0.0043 (18)	0.0036 (18)
C4	0.017 (2)	0.038 (3)	0.024 (2)	0.0016 (19)	0.0113 (19)	−0.0002 (19)

Geometric parameters (Å, º)

Rb1—O1^i	2.847 (4)	O2—C1	1.265 (6)
Rb1—O1^ii	2.859 (4)	O1—C1	1.240 (5)
Rb1—O2	2.927 (4)	O3—H1	0.94 (2)
Rb1—O3^iii	2.980 (4)	O3—H2	0.94 (2)
Rb1—O2^iii	3.005 (4)	C1—C2	1.511 (6)
Rb1—O3	3.136 (4)	C2—C3	1.395 (6)
Rb1—O3^iv	3.172 (4)	C2—C4	1.396 (7)
Rb1—O3^v	3.327 (4)	C3—C4^vii	1.389 (6)
Rb1—Rb1^iii	3.9531 (5)	C3—H3	0.9300
Rb1—Rb1^vi	3.9531 (5)	C4—H4	0.9300
O1^i—Rb1—O1^ii	87.71 (9)	O2^iii—Rb1—Rb1^vi	132.62 (7)
O1^i—Rb1—O2	84.44 (11)	O3—Rb1—Rb1^vi	48.03 (8)
O1^ii—Rb1—O2	144.07 (11)	O3^iv—Rb1—Rb1^vi	85.57 (8)
O1^i—Rb1—O3^iii	138.19 (12)	O3^v—Rb1—Rb1^vi	87.93 (8)
O1^ii—Rb1—O3^iii	83.16 (11)	C3^iii—Rb1—Rb1^vi	112.32 (8)
O2—Rb1—O3^iii	124.43 (11)	C1^iii—Rb1—Rb1^vi	116.47 (7)
O1^i—Rb1—O2^iii	144.59 (10)	Rb1^iii—Rb1—Rb1^vi	180.0
O1^ii—Rb1—O2^iii	82.84 (11)	O1^i—Rb1—H2	94.3 (8)
O2—Rb1—O2^iii	83.56 (9)	O1^ii—Rb1—H2	130.9 (10)
O3^iii—Rb1—O2^iii	74.42 (11)	O2—Rb1—H2	84.7 (9)
O1^i—Rb1—O3	80.62 (10)	O3^iii—Rb1—H2	63.3 (5)
O1^ii—Rb1—O3	139.66 (11)	O2^iii—Rb1—H2	117.5 (10)
O2—Rb1—O3	73.22 (11)	O3—Rb1—H2	17.2 (4)
O3^iii—Rb1—O3	80.49 (9)	O3^iv—Rb1—H2	66.0 (12)
O2^iii—Rb1—O3	126.75 (10)	O3^v—Rb1—H2	68.1 (12)
O1^i—Rb1—O3^iv	64.31 (11)	C3^iii—Rb1—H2	160.5 (12)
O1^ii—Rb1—O3^iv	71.05 (11)	C1^iii—Rb1—H2	122.1 (11)
O2—Rb1—O3^iv	133.89 (11)	Rb1^iii—Rb1—H2	114.8 (5)
O3^iii—Rb1—O3^iv	74.15 (13)	Rb1^vi—Rb1—H2	65.2 (5)
O2^iii—Rb1—O3^iv	141.01 (10)	C1—O2—Rb1	146.7 (3)
O3—Rb1—O3^iv	69.08 (13)	C1—O2—Rb1^vi	115.1 (3)
O1^i—Rb1—O3^v	133.23 (11)	Rb1—O2—Rb1^vi	83.56 (9)
O1^ii—Rb1—O3^v	137.05 (11)	C1—O1—Rb1^viii	134.8 (3)
O2—Rb1—O3^v	52.20 (10)	C1—O1—Rb1^ix	129.7 (3)
O3^iii—Rb1—O3^v	73.37 (11)	Rb1^viii—O1—Rb1^ix	87.71 (9)
O2^iii—Rb1—O3^v	56.66 (10)	Rb1^vi—O3—Rb1	80.49 (9)
O3—Rb1—O3^v	71.49 (11)	Rb1^vi—O3—Rb1^iv	105.85 (13)
O3^iv—Rb1—O3^v	132.01 (12)	Rb1—O3—Rb1^iv	110.92 (12)
O1^i—Rb1—C3^iii	96.64 (11)	Rb1^vi—O3—Rb1^x	109.34 (13)
O1^ii—Rb1—C3^iii	65.79 (11)	Rb1—O3—Rb1^x	105.62 (12)
O2—Rb1—C3^iii	80.36 (11)	Rb1^iv—O3—Rb1^x	132.45 (12)
O3^iii—Rb1—C3^iii	116.00 (12)	Rb1^vi—O3—H1	95 (4)
O2^iii—Rb1—C3^iii	48.48 (10)	Rb1—O3—H1	170 (4)
O3—Rb1—C3^iii	153.57 (11)	Rb1^iv—O3—H1	79 (3)
O3^iv—Rb1—C3^iii	133.38 (10)	Rb1^x—O3—H1	67 (4)
O3^v—Rb1—C3^iii	92.74 (10)	Rb1^vi—O3—H2	165 (5)
O1^i—Rb1—C1^iii	130.00 (11)	Rb1—O3—H2	84 (5)
O1^ii—Rb1—C1^iii	91.36 (10)	Rb1^iv—O3—H2	79 (4)
O2—Rb1—C1^iii	68.00 (11)	Rb1^x—O3—H2	75 (4)
O3^iii—Rb1—C1^iii	91.05 (11)	H1—O3—H2	100 (6)
O2^iii—Rb1—C1^iii	17.94 (10)	O1—C1—O2	123.7 (4)
O3—Rb1—C1^iii	125.41 (10)	O1—C1—C2	119.0 (4)
O3^iv—Rb1—C1^iii	157.95 (11)	O2—C1—C2	117.2 (4)
O3^v—Rb1—C1^iii	54.59 (10)	O1—C1—Rb1^vi	133.4 (3)
C3^iii—Rb1—C1^iii	39.96 (10)	O2—C1—Rb1^vi	47.0 (2)
O1^i—Rb1—Rb1^iii	133.73 (7)	C2—C1—Rb1^vi	88.1 (2)
O1^ii—Rb1—Rb1^iii	46.02 (8)	C3—C2—C4	119.0 (4)
O2—Rb1—Rb1^iii	130.95 (8)	C3—C2—C1	121.4 (4)
O3^iii—Rb1—Rb1^iii	51.47 (8)	C4—C2—C1	119.6 (4)
O2^iii—Rb1—Rb1^iii	47.38 (7)	C4^vii—C3—C2	120.2 (4)
O3—Rb1—Rb1^iii	131.97 (8)	C4^vii—C3—Rb1^vi	124.8 (3)
O3^iv—Rb1—Rb1^iii	94.43 (8)	C2—C3—Rb1^vi	90.8 (3)
O3^v—Rb1—Rb1^iii	92.07 (8)	C4^vii—C3—H3	119.9
C3^iii—Rb1—Rb1^iii	67.68 (8)	C2—C3—H3	119.9
C1^iii—Rb1—Rb1^iii	63.53 (7)	Rb1^vi—C3—H3	54.0
O1^i—Rb1—Rb1^vi	46.27 (7)	C3^vii—C4—C2	120.8 (4)
O1^ii—Rb1—Rb1^vi	133.98 (8)	C3^vii—C4—H4	119.6
O2—Rb1—Rb1^vi	49.05 (7)	C2—C4—H4	119.6
O3^iii—Rb1—Rb1^vi	128.53 (8)

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, −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^x	0.94 (2)	1.86 (3)	2.775 (5)	164 (5)
O3—H2···O2^v	0.94 (2)	2.15 (4)	3.018 (6)	153 (6)
O3—H2···O1^v	0.94 (2)	2.42 (5)	3.215 (6)	141 (6)

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