Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680602928X/ng2059sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680602928X/ng2059Isup2.hkl |
CCDC reference: 621420
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (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
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.
[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) Å3 | 0.4 × 0.3 × 0.07 mm |
Z = 2 |
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 on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.042 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.103 | w = 1/[σ2(Fo2) + (0.0625P)2] where P = (Fo2 + 2Fc2)/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+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.015 (3) |
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. |
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)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
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) |
Rb1—O1i | 2.847 (4) | O2—C1 | 1.265 (6) |
Rb1—O1ii | 2.859 (4) | O1—C1 | 1.240 (5) |
Rb1—O2 | 2.927 (4) | O3—H1 | 0.94 (2) |
Rb1—O3iii | 2.980 (4) | O3—H2 | 0.94 (2) |
Rb1—O2iii | 3.005 (4) | C1—C2 | 1.511 (6) |
Rb1—O3 | 3.136 (4) | C2—C3 | 1.395 (6) |
Rb1—O3iv | 3.172 (4) | C2—C4 | 1.396 (7) |
Rb1—O3v | 3.327 (4) | C3—C4vii | 1.389 (6) |
Rb1—Rb1iii | 3.9531 (5) | C3—H3 | 0.9300 |
Rb1—Rb1vi | 3.9531 (5) | C4—H4 | 0.9300 |
O1i—Rb1—O1ii | 87.71 (9) | O2iii—Rb1—Rb1vi | 132.62 (7) |
O1i—Rb1—O2 | 84.44 (11) | O3—Rb1—Rb1vi | 48.03 (8) |
O1ii—Rb1—O2 | 144.07 (11) | O3iv—Rb1—Rb1vi | 85.57 (8) |
O1i—Rb1—O3iii | 138.19 (12) | O3v—Rb1—Rb1vi | 87.93 (8) |
O1ii—Rb1—O3iii | 83.16 (11) | C3iii—Rb1—Rb1vi | 112.32 (8) |
O2—Rb1—O3iii | 124.43 (11) | C1iii—Rb1—Rb1vi | 116.47 (7) |
O1i—Rb1—O2iii | 144.59 (10) | Rb1iii—Rb1—Rb1vi | 180.0 |
O1ii—Rb1—O2iii | 82.84 (11) | O1i—Rb1—H2 | 94.3 (8) |
O2—Rb1—O2iii | 83.56 (9) | O1ii—Rb1—H2 | 130.9 (10) |
O3iii—Rb1—O2iii | 74.42 (11) | O2—Rb1—H2 | 84.7 (9) |
O1i—Rb1—O3 | 80.62 (10) | O3iii—Rb1—H2 | 63.3 (5) |
O1ii—Rb1—O3 | 139.66 (11) | O2iii—Rb1—H2 | 117.5 (10) |
O2—Rb1—O3 | 73.22 (11) | O3—Rb1—H2 | 17.2 (4) |
O3iii—Rb1—O3 | 80.49 (9) | O3iv—Rb1—H2 | 66.0 (12) |
O2iii—Rb1—O3 | 126.75 (10) | O3v—Rb1—H2 | 68.1 (12) |
O1i—Rb1—O3iv | 64.31 (11) | C3iii—Rb1—H2 | 160.5 (12) |
O1ii—Rb1—O3iv | 71.05 (11) | C1iii—Rb1—H2 | 122.1 (11) |
O2—Rb1—O3iv | 133.89 (11) | Rb1iii—Rb1—H2 | 114.8 (5) |
O3iii—Rb1—O3iv | 74.15 (13) | Rb1vi—Rb1—H2 | 65.2 (5) |
O2iii—Rb1—O3iv | 141.01 (10) | C1—O2—Rb1 | 146.7 (3) |
O3—Rb1—O3iv | 69.08 (13) | C1—O2—Rb1vi | 115.1 (3) |
O1i—Rb1—O3v | 133.23 (11) | Rb1—O2—Rb1vi | 83.56 (9) |
O1ii—Rb1—O3v | 137.05 (11) | C1—O1—Rb1viii | 134.8 (3) |
O2—Rb1—O3v | 52.20 (10) | C1—O1—Rb1ix | 129.7 (3) |
O3iii—Rb1—O3v | 73.37 (11) | Rb1viii—O1—Rb1ix | 87.71 (9) |
O2iii—Rb1—O3v | 56.66 (10) | Rb1vi—O3—Rb1 | 80.49 (9) |
O3—Rb1—O3v | 71.49 (11) | Rb1vi—O3—Rb1iv | 105.85 (13) |
O3iv—Rb1—O3v | 132.01 (12) | Rb1—O3—Rb1iv | 110.92 (12) |
O1i—Rb1—C3iii | 96.64 (11) | Rb1vi—O3—Rb1x | 109.34 (13) |
O1ii—Rb1—C3iii | 65.79 (11) | Rb1—O3—Rb1x | 105.62 (12) |
O2—Rb1—C3iii | 80.36 (11) | Rb1iv—O3—Rb1x | 132.45 (12) |
O3iii—Rb1—C3iii | 116.00 (12) | Rb1vi—O3—H1 | 95 (4) |
O2iii—Rb1—C3iii | 48.48 (10) | Rb1—O3—H1 | 170 (4) |
O3—Rb1—C3iii | 153.57 (11) | Rb1iv—O3—H1 | 79 (3) |
O3iv—Rb1—C3iii | 133.38 (10) | Rb1x—O3—H1 | 67 (4) |
O3v—Rb1—C3iii | 92.74 (10) | Rb1vi—O3—H2 | 165 (5) |
O1i—Rb1—C1iii | 130.00 (11) | Rb1—O3—H2 | 84 (5) |
O1ii—Rb1—C1iii | 91.36 (10) | Rb1iv—O3—H2 | 79 (4) |
O2—Rb1—C1iii | 68.00 (11) | Rb1x—O3—H2 | 75 (4) |
O3iii—Rb1—C1iii | 91.05 (11) | H1—O3—H2 | 100 (6) |
O2iii—Rb1—C1iii | 17.94 (10) | O1—C1—O2 | 123.7 (4) |
O3—Rb1—C1iii | 125.41 (10) | O1—C1—C2 | 119.0 (4) |
O3iv—Rb1—C1iii | 157.95 (11) | O2—C1—C2 | 117.2 (4) |
O3v—Rb1—C1iii | 54.59 (10) | O1—C1—Rb1vi | 133.4 (3) |
C3iii—Rb1—C1iii | 39.96 (10) | O2—C1—Rb1vi | 47.0 (2) |
O1i—Rb1—Rb1iii | 133.73 (7) | C2—C1—Rb1vi | 88.1 (2) |
O1ii—Rb1—Rb1iii | 46.02 (8) | C3—C2—C4 | 119.0 (4) |
O2—Rb1—Rb1iii | 130.95 (8) | C3—C2—C1 | 121.4 (4) |
O3iii—Rb1—Rb1iii | 51.47 (8) | C4—C2—C1 | 119.6 (4) |
O2iii—Rb1—Rb1iii | 47.38 (7) | C4vii—C3—C2 | 120.2 (4) |
O3—Rb1—Rb1iii | 131.97 (8) | C4vii—C3—Rb1vi | 124.8 (3) |
O3iv—Rb1—Rb1iii | 94.43 (8) | C2—C3—Rb1vi | 90.8 (3) |
O3v—Rb1—Rb1iii | 92.07 (8) | C4vii—C3—H3 | 119.9 |
C3iii—Rb1—Rb1iii | 67.68 (8) | C2—C3—H3 | 119.9 |
C1iii—Rb1—Rb1iii | 63.53 (7) | Rb1vi—C3—H3 | 54.0 |
O1i—Rb1—Rb1vi | 46.27 (7) | C3vii—C4—C2 | 120.8 (4) |
O1ii—Rb1—Rb1vi | 133.98 (8) | C3vii—C4—H4 | 119.6 |
O2—Rb1—Rb1vi | 49.05 (7) | C2—C4—H4 | 119.6 |
O3iii—Rb1—Rb1vi | 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. |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H1···O2x | 0.94 (2) | 1.86 (3) | 2.775 (5) | 164 (5) |
O3—H2···O2v | 0.94 (2) | 2.15 (4) | 3.018 (6) | 153 (6) |
O3—H2···O1v | 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. |
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