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In the bimetallic coordination polymer [PtRbCl2(C12H7N2O4)(H2O)]n, the PtII atom has a square-planar configuration, with two cis-coordinated N atoms from a 2,2′-bipyridine-5,5′-dicarboxyl­ate ligand and two terminal Cl atoms. The carboxyl­ate groups are further connected to Rb ions, forming two-dimensional sheets, which again are linked together through Rb—Cl bonds, forming a three-dimensional structure. The bimetallic coordination polymer contains PtII sites with the same configuration as homogenous Pt-containing metal–organic complexes, which proved to be active species in C—H bond-activation reactions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807008902/sg2140sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807008902/sg2140Isup2.hkl
Contains datablock I

CCDC reference: 643085

Key indicators

  • Single-crystal X-ray study
  • T = 313 K
  • Mean [sigma](C-C) = 0.012 Å
  • H-atom completeness 78%
  • R factor = 0.032
  • wR factor = 0.090
  • Data-to-parameter ratio = 14.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.77 PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 100 Deg. PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 4 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.14 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 12 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.17 Ratio
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C12 H9 Cl2 N2 O5 Pt1 Rb1 Atom count from the _atom_site data: C12 H7 Cl2 N2 O5 Pt1 Rb1 ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.772 Tmax scaled 0.280 Tmin scaled 0.128 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C12 H9 Cl2 N2 O5 Pt Rb TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 24.00 24.00 0.00 H 18.00 14.00 4.00 Cl 4.00 4.00 0.00 N 4.00 4.00 0.00 O 10.00 10.00 0.00 Pt 2.00 2.00 0.00 Rb 2.00 2.00 0.00 PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 5 ALERT level G = General alerts; check 7 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 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2000); software used to prepare material for publication: SHELXL97.

poly[aqua(µ-5'-carboxy-2,2'-bipyridine-5- carboxylato)dichlororubidium(I)platinum(II)] top
Crystal data top
[PtRbCl2(C12H7N2O4)(H2O)]Z = 2
Mr = 612.67F(000) = 568
Triclinic, P1Dx = 2.666 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.8859 (10) ÅCell parameters from 2953 reflections
b = 9.4092 (10) Åθ = 2.2–26.0°
c = 10.0290 (11) ŵ = 12.73 mm1
α = 88.671 (1)°T = 313 K
β = 69.279 (1)°Cube, yellow
γ = 77.182 (1)°0.22 × 0.14 × 0.10 mm
V = 763.33 (14) Å3
Data collection top
Bruker D8 Apex II CCD
diffractometer
2953 independent reflections
Radiation source: fine-focus sealed tube2783 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.015
ω scansθmax = 26.0°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997)
h = 1010
Tmin = 0.166, Tmax = 0.362k = 1111
5890 measured reflectionsl = 1212
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.090H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0473P)2 + 5.767P]
where P = (Fo2 + 2Fc2)/3
2953 reflections(Δ/σ)max < 0.001
208 parametersΔρmax = 1.27 e Å3
0 restraintsΔρmin = 2.50 e Å3
Special details top

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 (Å2) top
xyzUiso*/Ueq
Pt10.14772 (3)0.38305 (3)0.32843 (3)0.02739 (11)
Cl10.3088 (2)0.2405 (3)0.4385 (2)0.0474 (5)
Cl20.3732 (3)0.4647 (3)0.1875 (3)0.0488 (5)
N10.0570 (7)0.3133 (6)0.4359 (6)0.0274 (12)
N20.0057 (7)0.5018 (6)0.2418 (6)0.0276 (12)
C10.1885 (9)0.3654 (8)0.3949 (8)0.0294 (15)
C20.3318 (9)0.3234 (9)0.4535 (9)0.0352 (17)
H20.41840.35740.42090.042*
C30.3493 (10)0.2286 (9)0.5633 (9)0.0383 (18)
H30.44770.19860.60500.046*
C40.2197 (9)0.1793 (8)0.6101 (8)0.0325 (16)
C50.0740 (9)0.2222 (8)0.5424 (8)0.0322 (16)
H50.01520.18690.57140.039*
C60.1585 (9)0.4729 (8)0.2846 (7)0.0276 (14)
C70.2757 (10)0.5415 (9)0.2294 (8)0.0352 (17)
H70.37820.51770.25750.042*
C80.2383 (10)0.6468 (9)0.1315 (9)0.0375 (18)
H80.31570.69440.09300.045*
C90.0874 (10)0.6797 (8)0.0921 (8)0.0317 (16)
C100.0291 (9)0.6051 (8)0.1465 (8)0.0314 (15)
H100.13300.62630.11700.038*
C110.7617 (11)1.0860 (9)0.2636 (8)0.0375 (18)
C120.0372 (11)0.7909 (8)0.0165 (9)0.0371 (18)
O10.6227 (8)1.0803 (7)0.1827 (6)0.0480 (15)
O20.8977 (8)1.0217 (8)0.2500 (7)0.0529 (17)
O30.1007 (8)0.8071 (7)0.0641 (7)0.0527 (16)
Rb10.41380 (13)0.87977 (12)0.11828 (11)0.0620 (3)
O50.2476 (11)1.0206 (9)0.2937 (9)0.073 (2)
O40.1591 (8)0.8599 (7)0.0509 (6)0.0482 (15)
H40.15900.91980.10180.072*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.02187 (16)0.03184 (17)0.03074 (16)0.00765 (11)0.01176 (11)0.01008 (11)
Cl10.0300 (10)0.0670 (14)0.0501 (11)0.0093 (9)0.0225 (9)0.0253 (10)
Cl20.0285 (10)0.0585 (13)0.0631 (13)0.0198 (9)0.0163 (9)0.0248 (11)
N10.027 (3)0.028 (3)0.027 (3)0.005 (2)0.011 (2)0.011 (2)
N20.024 (3)0.026 (3)0.032 (3)0.008 (2)0.009 (2)0.010 (2)
C10.033 (4)0.028 (3)0.030 (4)0.007 (3)0.016 (3)0.009 (3)
C20.026 (4)0.042 (4)0.043 (4)0.013 (3)0.017 (3)0.020 (3)
C30.028 (4)0.045 (5)0.043 (4)0.014 (3)0.013 (3)0.019 (4)
C40.033 (4)0.031 (4)0.031 (4)0.007 (3)0.009 (3)0.010 (3)
C50.029 (4)0.035 (4)0.034 (4)0.007 (3)0.014 (3)0.016 (3)
C60.029 (4)0.028 (3)0.027 (3)0.007 (3)0.011 (3)0.008 (3)
C70.028 (4)0.041 (4)0.041 (4)0.013 (3)0.015 (3)0.017 (3)
C80.033 (4)0.039 (4)0.044 (4)0.005 (3)0.021 (3)0.019 (3)
C90.038 (4)0.026 (3)0.028 (3)0.004 (3)0.011 (3)0.007 (3)
C100.030 (4)0.028 (4)0.034 (4)0.009 (3)0.009 (3)0.011 (3)
C110.045 (5)0.035 (4)0.032 (4)0.012 (3)0.012 (3)0.014 (3)
C120.043 (5)0.029 (4)0.037 (4)0.006 (3)0.013 (4)0.009 (3)
O10.041 (3)0.056 (4)0.043 (3)0.019 (3)0.009 (3)0.028 (3)
O20.040 (3)0.063 (4)0.051 (4)0.008 (3)0.016 (3)0.035 (3)
O30.044 (4)0.048 (4)0.060 (4)0.017 (3)0.009 (3)0.027 (3)
Rb10.0545 (6)0.0659 (6)0.0600 (6)0.0145 (5)0.0138 (5)0.0088 (5)
O50.075 (5)0.075 (5)0.077 (5)0.019 (4)0.036 (4)0.020 (4)
O40.052 (4)0.048 (3)0.043 (3)0.009 (3)0.018 (3)0.030 (3)
Geometric parameters (Å, º) top
Pt1—N21.995 (6)C7—C81.388 (10)
Pt1—N12.003 (6)C7—H70.9300
Pt1—Cl22.287 (2)C8—C91.361 (11)
Pt1—Cl12.2936 (19)C8—H80.9300
Pt1—Rb1i3.9867 (11)C9—C101.386 (10)
Cl1—Rb1i3.316 (3)C9—C121.514 (10)
Cl2—Rb1i3.320 (3)C10—H100.9300
N1—C51.341 (9)C11—O11.227 (10)
N1—C11.361 (9)C11—O21.278 (10)
N2—C101.354 (9)C11—C4iii1.505 (10)
N2—C61.360 (9)C11—Rb1iv3.579 (8)
C1—C21.344 (11)C12—O31.190 (10)
C1—C61.475 (9)C12—O41.286 (10)
C2—C31.388 (10)O1—Rb12.841 (6)
C2—H20.9300O1—Rb1iv2.943 (6)
C3—C41.377 (11)O3—Rb12.874 (7)
C3—H30.9300Rb1—O52.809 (8)
C4—C51.377 (11)Rb1—O4v3.003 (7)
C4—C11ii1.505 (10)Rb1—C11iv3.579 (8)
C5—H50.9300Rb1—Rb1iv4.178 (2)
C6—C71.378 (10)O4—H40.752
N2—Pt1—N180.8 (2)O3—C12—C9122.3 (7)
N2—Pt1—Cl294.61 (17)O4—C12—C9111.8 (7)
N1—Pt1—Cl2174.52 (17)C11—O1—Rb1138.4 (6)
N2—Pt1—Cl1175.99 (17)C11—O1—Rb1iv111.5 (5)
N1—Pt1—Cl195.19 (17)Rb1—O1—Rb1iv92.47 (16)
Cl2—Pt1—Cl189.40 (8)C12—O3—Rb1167.2 (6)
N2—Pt1—Rb1i126.37 (17)O5—Rb1—O190.7 (2)
N1—Pt1—Rb1i124.24 (17)O5—Rb1—O367.1 (2)
Cl2—Pt1—Rb1i56.36 (6)O1—Rb1—O3152.22 (18)
Cl1—Pt1—Rb1i56.27 (6)O5—Rb1—O1iv135.0 (2)
Pt1—Cl1—Rb1i88.62 (7)O1—Rb1—O1iv87.53 (16)
Pt1—Cl2—Rb1i88.65 (7)O3—Rb1—O1iv96.63 (19)
C5—N1—C1118.7 (6)O5—Rb1—O4v72.0 (2)
C5—N1—Pt1125.9 (5)O1—Rb1—O4v82.89 (18)
C1—N1—Pt1115.4 (5)O3—Rb1—O4v74.73 (19)
C10—N2—C6118.7 (6)O1iv—Rb1—O4v63.21 (17)
C10—N2—Pt1126.3 (5)O5—Rb1—Cl1i79.52 (19)
C6—N2—Pt1115.0 (4)O1—Rb1—Cl1i75.97 (14)
C2—C1—N1122.0 (6)O3—Rb1—Cl1i113.71 (16)
C2—C1—C6124.4 (7)O1iv—Rb1—Cl1i142.42 (13)
N1—C1—C6113.6 (6)O4v—Rb1—Cl1i144.11 (11)
C1—C2—C3119.3 (7)O5—Rb1—Cl2i122.09 (19)
C1—C2—H2120.4O1—Rb1—Cl2i112.22 (14)
C3—C2—H2120.4O3—Rb1—Cl2i94.19 (14)
C4—C3—C2119.5 (7)O1iv—Rb1—Cl2i99.83 (14)
C4—C3—H3120.2O4v—Rb1—Cl2i157.65 (12)
C2—C3—H3120.2Cl1i—Rb1—Cl2i58.09 (6)
C5—C4—C3118.5 (7)O5—Rb1—C11iv123.1 (2)
C5—C4—C11ii120.4 (7)O1—Rb1—C11iv102.77 (19)
C3—C4—C11ii121.1 (7)O3—Rb1—C11iv78.2 (2)
N1—C5—C4122.0 (7)O1iv—Rb1—C11iv18.61 (18)
N1—C5—H5119.0O4v—Rb1—C11iv55.86 (16)
C4—C5—H5119.0Cl1i—Rb1—C11iv157.30 (14)
N2—C6—C7121.8 (6)Cl2i—Rb1—C11iv103.34 (14)
N2—C6—C1114.9 (6)O5—Rb1—Pt1i114.56 (19)
C7—C6—C1123.4 (7)O1—Rb1—Pt1i78.75 (13)
C6—C7—C8118.9 (7)O3—Rb1—Pt1i124.76 (14)
C6—C7—H7120.5O1iv—Rb1—Pt1i109.10 (13)
C8—C7—H7120.5O4v—Rb1—Pt1i160.48 (14)
C9—C8—C7119.4 (7)Cl1i—Rb1—Pt1i35.11 (3)
C9—C8—H8120.3Cl2i—Rb1—Pt1i34.99 (4)
C7—C8—H8120.3C11iv—Rb1—Pt1i122.19 (14)
C8—C9—C10119.9 (7)O5—Rb1—Rb1iv120.40 (18)
C8—C9—C12122.2 (7)O1—Rb1—Rb1iv44.74 (13)
C10—C9—C12117.8 (7)O3—Rb1—Rb1iv133.07 (15)
N2—C10—C9121.2 (7)O1iv—Rb1—Rb1iv42.79 (12)
N2—C10—H10119.4O4v—Rb1—Rb1iv66.31 (13)
C9—C10—H10119.4Cl1i—Rb1—Rb1iv113.17 (6)
O1—C11—O2126.0 (7)Cl2i—Rb1—Rb1iv112.17 (6)
O1—C11—C4iii119.3 (7)C11iv—Rb1—Rb1iv58.84 (14)
O2—C11—C4iii114.7 (7)Pt1i—Rb1—Rb1iv95.61 (4)
O1—C11—Rb1iv49.9 (4)C12—O4—Rb1v124.2 (5)
O2—C11—Rb1iv86.9 (5)C12—O4—H4127.5
C4iii—C11—Rb1iv140.0 (5)Rb1v—O4—H473.7 (5)
O3—C12—O4125.9 (8)
Cl2—Pt1—Cl1—Rb1i48.76 (8)Pt1—N2—C10—C9179.2 (5)
N2—Pt1—Cl2—Rb1i131.37 (18)C8—C9—C10—N21.8 (12)
Cl1—Pt1—Cl2—Rb1i48.69 (8)C12—C9—C10—N2178.6 (7)
N2—Pt1—N1—C5174.9 (7)C8—C9—C12—O3170.6 (8)
Cl1—Pt1—N1—C54.8 (6)C10—C9—C12—O36.2 (12)
Rb1i—Pt1—N1—C557.0 (7)C8—C9—C12—O47.9 (11)
N2—Pt1—N1—C14.9 (5)C10—C9—C12—O4175.3 (7)
Cl1—Pt1—N1—C1175.4 (5)O2—C11—O1—Rb175.2 (12)
Rb1i—Pt1—N1—C1123.2 (5)C4iii—C11—O1—Rb1106.6 (8)
N1—Pt1—N2—C10175.6 (6)Rb1iv—C11—O1—Rb1120.8 (8)
Cl2—Pt1—N2—C107.4 (6)O2—C11—O1—Rb1iv45.7 (11)
Rb1i—Pt1—N2—C1058.3 (7)C4iii—C11—O1—Rb1iv132.5 (6)
N1—Pt1—N2—C64.7 (5)O4—C12—O3—Rb1105 (2)
Cl2—Pt1—N2—C6172.3 (5)C9—C12—O3—Rb176 (3)
Rb1i—Pt1—N2—C6121.4 (5)C11—O1—Rb1—O598.1 (8)
C5—N1—C1—C22.9 (11)Rb1iv—O1—Rb1—O5135.0 (2)
Pt1—N1—C1—C2177.3 (6)C11—O1—Rb1—O3133.6 (8)
C5—N1—C1—C6175.7 (6)Rb1iv—O1—Rb1—O399.6 (4)
Pt1—N1—C1—C64.1 (8)C11—O1—Rb1—O1iv126.9 (9)
N1—C1—C2—C32.7 (13)Rb1iv—O1—Rb1—O1iv0.0
C6—C1—C2—C3175.8 (7)C11—O1—Rb1—O4v169.8 (8)
C1—C2—C3—C40.0 (13)Rb1iv—O1—Rb1—O4v63.30 (17)
C2—C3—C4—C52.2 (12)C11—O1—Rb1—Cl1i19.1 (8)
C2—C3—C4—C11ii175.1 (8)Rb1iv—O1—Rb1—Cl1i145.93 (16)
C1—N1—C5—C40.5 (11)C11—O1—Rb1—Cl2i27.3 (8)
Pt1—N1—C5—C4179.7 (6)Rb1iv—O1—Rb1—Cl2i99.61 (15)
C3—C4—C5—N12.0 (12)C11—O1—Rb1—C11iv137.6 (7)
C11ii—C4—C5—N1175.4 (7)Rb1iv—O1—Rb1—C11iv10.8 (2)
C10—N2—C6—C72.5 (11)C11—O1—Rb1—Pt1i16.8 (8)
Pt1—N2—C6—C7177.2 (6)Rb1iv—O1—Rb1—Pt1i110.03 (14)
C10—N2—C6—C1176.5 (6)C11—O1—Rb1—Rb1iv126.9 (9)
Pt1—N2—C6—C13.8 (8)C12—O3—Rb1—O5114 (3)
C2—C1—C6—N2178.8 (7)C12—O3—Rb1—O175 (3)
N1—C1—C6—N20.2 (9)C12—O3—Rb1—O1iv22 (3)
C2—C1—C6—C70.2 (12)C12—O3—Rb1—O4v38 (3)
N1—C1—C6—C7178.8 (7)C12—O3—Rb1—Cl1i179 (2)
N2—C6—C7—C82.3 (12)C12—O3—Rb1—Cl2i123 (3)
C1—C6—C7—C8176.6 (7)C12—O3—Rb1—C11iv20 (3)
C6—C7—C8—C90.0 (13)C12—O3—Rb1—Pt1i141 (2)
C7—C8—C9—C102.0 (12)C12—O3—Rb1—Rb1iv3 (3)
C7—C8—C9—C12178.7 (8)O3—C12—O4—Rb1v98.3 (9)
C6—N2—C10—C90.5 (11)C9—C12—O4—Rb1v83.3 (7)
Symmetry codes: (i) x+1, y+1, z; (ii) x1, y1, z+1; (iii) x+1, y+1, z1; (iv) x+1, y+2, z; (v) x, y+2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C2—H2···Cl1vi0.932.833.505 (8)131
C7—H7···Cl2vi0.932.693.518 (8)149
Symmetry code: (vi) x1, y, z.
 

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