Download citation
Download citation
link to html
The intradimer Pt—Pt distance [3.0928 (9) Å] in the title compound, [Pt2(μ-C5H9O2)2(NH3)4](ClO4)2·C5H10O2, is much longer than that reported for [Pt2(μ-C5H9O2)2(NH3)4](SO4)·H2O [2.9011 (9) Å; Sakai, Ishigami, Yokokawa, Kajiwara & Ito (2003). Acta Cryst. E59, m443–m445]. The complex cation has a crystallographic mirror plane perpendicular to the Pt—Pt bond. The crystal packing is stabilized by both the hydro­philic and hydro­phobic layers, which stack alternately along the c axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803026503/ob6323sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803026503/ob6323Isup2.hkl
Contains datablock I

CCDC reference: 227765

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.019 Å
  • H-atom completeness 98%
  • Disorder in solvent or counterion
  • R factor = 0.041
  • wR factor = 0.079
  • Data-to-parameter ratio = 20.1

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ..... = 2 PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.80 Ratio PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors .... C6 PLAT430_ALERT_2_B Short Inter D...A Contact O8 .. O12 = 2.73 Ang.
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.391 0.563 Tmin and Tmax expected: 0.330 0.621 RR = 1.307 Please check that your absorption correction is appropriate. PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.30 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 1.10 PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Pt1 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C2 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... C9 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... C10 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl1 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl2 PLAT301_ALERT_3_C Main Residue Disorder ......................... 13.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 31.00 Perc. PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 19 PLAT480_ALERT_4_C Long H...A H-Bond Reported H2C .. O8 = 2.93 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H2B .. O9 = 2.69 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H1A .. O12 = 2.64 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 12 PLAT728_ALERT_1_C D-H..A Calc 143.99, Rep 145.00, Dev. 1.01 Deg. N2 -H2C -O5 1.555 1.555 2.565 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 Cl O4 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 Cl O4
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:C15 H40 Cl2 N4 O14 Pt2 Atom count from the _atom_site data: C15 H39 Cl2 N4 O14 Pt2 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 1.103 Tmax scaled 0.621 Tmin scaled 0.432 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 4 From the CIF: _chemical_formula_sum C15 H40 Cl2 N4 O14 Pt2 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 60.00 60.00 0.00 H 160.00 156.00 4.00 Cl 8.00 8.00 0.00 N 16.00 16.00 0.00 O 56.00 56.00 0.00 Pt 8.00 8.00 0.00
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 22 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 7 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 12 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: KENX (Sakai, 2002); software used to prepare material for publication: SHELXL97 and TEXSAN (Molecular Structure Corporation, 2001), KENX, and ORTEP (Johnson, 1976).

Di-µ-pivalato-bis[cis-diammineplatinum(II)] bis(perchlorate) pivalic acid top
Crystal data top
[Pt2(C5H9O2)2(NH3)4](ClO4)2·C5H10O2F(000) = 1840
Mr = 961.59? # Insert any comments here.
Monoclinic, C2/mDx = 2.124 Mg m3
Hall symbol: -C 2yMo Kα radiation, λ = 0.71073 Å
a = 18.194 (4) ÅCell parameters from 3676 reflections
b = 9.874 (2) Åθ = 7.0–19.9°
c = 18.987 (4) ŵ = 9.54 mm1
β = 118.155 (5)°T = 296 K
V = 3007.4 (10) Å3Prism, colorless
Z = 40.2 × 0.1 × 0.05 mm
Data collection top
Bruker SMART APEX CCD-detector
diffractometer
3676 independent reflections
Radiation source: fine-focus sealed tube2271 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.064
Detector resolution: 8.366 pixels mm-1θmax = 27.6°, θmin = 2.2°
ω scansh = 2323
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 1112
Tmin = 0.391, Tmax = 0.563l = 1624
11137 measured reflections
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)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.079H-atom parameters constrained
S = 0.86 w = 1/[σ2(Fo2) + (0.0237P)2]
where P = (Fo2 + 2Fc2)/3
3676 reflections(Δ/σ)max < 0.001
183 parametersΔρmax = 1.43 e Å3
42 restraintsΔρmin = 0.88 e Å3
Special details top

Experimental. The first 50 frames were rescanned at the end of data collection to evaluate any possible decay phenomenon. Since it was judged to be negligible, no decay correction was applied to the data.

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.

Mean-plane data from final SHELXL refinement run:-

Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane)

- 0.9268 (0.0428) x - 9.1605 (0.0093) y + 6.6472 (0.0439) z = 0.5453 (0.0139)

* -0.0135 (0.0033) O1 * 0.0139 (0.0034) O2 * -0.0140 (0.0034) N1 * 0.0136 (0.0033) N2 0.1054 (0.0033) Pt1 2.9746 (0.0036) Pt1_$10

Rms deviation of fitted atoms = 0.0137

- 0.9268 (0.0428) x + 9.1605 (0.0093) y + 6.6472 (0.0439) z = 0.5453 (0.0139)

Angle to previous plane (with approximate e.s.d.) = 43.84 (0.14)

* -0.0135 (0.0033) O1_$10 * 0.0139 (0.0034) O2_$10 * -0.0140 (0.0033) N1_$10 * 0.0136 (0.0033) N2_$10 0.1054 (0.0033) Pt1_$10 2.9746 (0.0036) Pt1

Rms deviation of fitted atoms = 0.0137

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*/UeqOcc. (<1)
Pt10.03989 (2)0.15661 (3)0.31927 (2)0.03594 (11)
Cl10.13669 (19)0.50000.4445 (2)0.0573 (9)
Cl20.1751 (2)0.0068 (13)0.4114 (2)0.0577 (15)0.50
O10.0734 (4)0.1138 (6)0.2266 (3)0.0504 (16)
O20.0973 (4)0.1130 (6)0.2534 (3)0.0489 (16)
O30.1334 (9)0.50000.2168 (8)0.157 (7)
O40.0793 (7)0.50000.2981 (7)0.106 (4)
O50.1061 (6)0.5254 (16)0.3887 (5)0.087 (2)*0.50
O60.2250 (4)0.512 (2)0.4056 (5)0.087 (2)*0.50
O70.0995 (7)0.5804 (11)0.5130 (6)0.087 (2)*0.50
O80.1157 (8)0.3585 (8)0.4687 (7)0.087 (2)*0.50
O90.0886 (5)0.011 (3)0.4612 (6)0.114 (3)*0.50
O100.2180 (7)0.0406 (15)0.4522 (7)0.114 (3)*0.50
O110.1938 (9)0.0758 (13)0.3438 (7)0.114 (3)*0.50
O120.2053 (10)0.1400 (12)0.3831 (9)0.114 (3)*0.50
N10.1508 (4)0.2199 (8)0.4040 (4)0.052 (2)
H1A0.19080.18550.39490.078*
H1B0.15820.19240.45150.078*
H1C0.15290.30990.40320.078*
N20.0173 (4)0.2185 (8)0.3828 (4)0.057 (2)
H2A0.01720.20830.43470.086*
H2B0.06300.16910.36920.086*
H2C0.03130.30540.37250.086*
C10.1025 (7)0.00000.1993 (7)0.039 (3)
C20.1871 (7)0.00000.1197 (7)0.044 (3)
C3A0.2518 (13)0.00000.1417 (16)0.075 (4)*0.532 (10)
H3A10.24710.07940.17270.091*0.266 (5)
H3A20.24700.07930.17280.091*0.266 (5)
H3A30.30500.00010.09440.091*0.532 (10)
C3B0.1590 (18)0.00000.0622 (15)0.075 (4)*0.468 (10)
H3B10.15180.09160.04980.091*0.234 (5)
H3B20.19930.04450.01470.091*0.234 (5)
H3B30.10680.04710.08300.091*0.234 (5)
C4A0.1951 (12)0.1193 (15)0.0740 (11)0.075 (4)*0.532 (10)
H4A10.15230.12010.05800.091*0.532 (10)
H4A20.18960.19790.10590.091*0.532 (10)
H4A30.24880.12000.02740.091*0.532 (10)
C4B0.2330 (12)0.1195 (16)0.1144 (13)0.075 (4)*0.468 (10)
H4B10.25270.11580.15320.091*0.468 (10)
H4B20.27970.12620.06180.091*0.468 (10)
H4B30.19770.19720.12450.091*0.468 (10)
C50.1130 (8)0.00000.2357 (7)0.043 (3)
C60.1539 (9)0.00000.1813 (9)0.060 (4)
C70.2096 (8)0.1211 (12)0.1984 (9)0.124 (5)
H7A0.24080.11330.16950.185*
H7B0.24740.12570.25460.185*
H7C0.17640.20190.18200.185*
C80.0874 (11)0.00000.0990 (10)0.150 (10)
H8A0.10730.04010.06510.225*0.50
H8B0.04090.05140.09540.225*0.50
H8C0.07000.09140.08220.225*0.50
C90.0729 (11)0.50000.2308 (10)0.077 (5)
C100.0132 (9)0.50000.1588 (8)0.065 (4)
C110.0857 (11)0.50000.1804 (12)0.125 (7)
H11A0.13750.51630.13320.188*0.50
H11B0.07640.57000.21890.188*0.50
H11C0.08790.41370.20270.188*0.50
C120.0176 (7)0.3735 (10)0.1098 (6)0.093 (4)
H12A0.01260.29380.14070.139*
H12B0.02710.37570.09640.139*
H12C0.07000.37190.06160.139*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.03697 (19)0.03326 (18)0.03636 (19)0.0022 (2)0.01628 (14)0.00409 (19)
Cl10.043 (2)0.056 (2)0.067 (2)0.0000.0218 (18)0.000
Cl20.048 (2)0.062 (4)0.067 (3)0.016 (7)0.031 (2)0.035 (7)
O10.053 (4)0.034 (4)0.050 (4)0.001 (3)0.013 (3)0.005 (3)
O20.059 (4)0.041 (4)0.060 (4)0.001 (3)0.038 (3)0.002 (3)
O30.104 (11)0.26 (2)0.116 (12)0.0000.056 (10)0.000
O40.123 (10)0.088 (10)0.076 (8)0.0000.020 (8)0.000
N10.050 (5)0.057 (5)0.053 (5)0.005 (4)0.028 (4)0.012 (4)
N20.050 (5)0.070 (6)0.055 (5)0.003 (4)0.026 (4)0.021 (4)
C10.042 (8)0.038 (8)0.043 (8)0.0000.025 (6)0.000
C20.041 (8)0.038 (8)0.048 (8)0.0000.016 (6)0.000
C50.044 (8)0.048 (9)0.044 (8)0.0000.025 (7)0.000
C60.080 (11)0.060 (10)0.063 (10)0.0000.051 (9)0.000
C70.162 (13)0.091 (12)0.197 (15)0.032 (9)0.151 (13)0.021 (10)
C80.123 (17)0.28 (3)0.059 (13)0.0000.057 (13)0.000
C90.091 (14)0.083 (13)0.053 (11)0.0000.031 (11)0.000
C100.072 (11)0.030 (9)0.061 (10)0.0000.006 (8)0.000
C110.112 (16)0.097 (18)0.20 (2)0.0000.097 (16)0.000
C120.101 (9)0.061 (9)0.086 (9)0.002 (7)0.020 (7)0.019 (6)
Geometric parameters (Å, º) top
Pt1—N11.997 (6)N1—H1B0.8900
Pt1—O22.018 (5)N1—H1C0.8900
Pt1—N22.025 (6)N2—H2A0.8900
Pt1—O12.025 (6)N2—H2B0.8900
Pt1—Pt1i3.0928 (9)N2—H2C0.8900
Pt1—Pt1ii6.7816 (16)C3A—H3A10.9600
Cl1—O71.395 (8)C3A—H3A20.9600
Cl1—O61.421 (7)C3A—H3A30.9600
Cl1—O51.434 (7)C3B—H3B10.9600
Cl1—O81.464 (8)C3B—H3B20.9600
Cl2—O91.403 (7)C3B—H3B30.9600
Cl2—O101.415 (8)C4A—H4A10.9600
Cl2—O111.420 (8)C4A—H4A20.9600
Cl2—O121.429 (9)C4A—H4A30.9600
O1—C11.246 (7)C4B—H4B10.9600
O2—C51.237 (7)C4B—H4B20.9600
O3—C91.248 (18)C4B—H4B30.9600
O4—C91.227 (16)C7—H7A0.9600
C1—C21.568 (15)C7—H7B0.9600
C2—C3B1.407 (10)C7—H7C0.9600
C2—C4B1.421 (9)C8—H8A0.9600
C2—C3A1.422 (10)C8—H8B0.9600
C2—C4A1.429 (9)C8—H8C0.9600
C5—C61.531 (16)C11—H11A0.9600
C6—C81.457 (19)C11—H11B0.9600
C6—C71.501 (12)C11—H11C0.9600
C9—C101.52 (2)C12—H12A0.9600
C10—C121.538 (12)C12—H12B0.9600
C10—C111.56 (2)C12—H12C0.9600
N1—H1A0.8900
N1—Pt1—O286.8 (3)H1A—N1—H1C109.5
N1—Pt1—N292.0 (3)H1B—N1—H1C109.5
O2—Pt1—N2174.7 (3)Pt1—N2—H2A109.5
N1—Pt1—O1173.1 (3)Pt1—N2—H2B109.5
O2—Pt1—O191.7 (2)H2A—N2—H2B109.5
N2—Pt1—O188.9 (3)Pt1—N2—H2C109.5
N1—Pt1—Pt1i108.2 (2)H2A—N2—H2C109.5
O2—Pt1—Pt1i77.68 (16)H2B—N2—H2C109.5
N2—Pt1—Pt1i107.6 (2)C2—C3A—H3A1109.5
O1—Pt1—Pt1i77.96 (16)C2—C3A—H3A2109.5
N1—Pt1—Pt1ii71.8 (2)H3A1—C3A—H3A2109.5
O2—Pt1—Pt1ii102.32 (16)C2—C3A—H3A3109.5
N2—Pt1—Pt1ii72.4 (2)H3A1—C3A—H3A3109.5
O1—Pt1—Pt1ii102.04 (16)H3A2—C3A—H3A3109.5
Pt1i—Pt1—Pt1ii180.00 (3)C2—C3B—H3B1109.5
O7—Cl1—O6111.7 (7)C2—C3B—H3B2109.5
O7—Cl1—O5113.7 (7)H3B1—C3B—H3B2109.5
O6—Cl1—O5109.9 (6)C2—C3B—H3B3109.5
O7—Cl1—O8108.1 (7)H3B1—C3B—H3B3109.5
O6—Cl1—O8107.7 (9)H3B2—C3B—H3B3109.5
O5—Cl1—O8105.3 (7)C2—C4A—H4A1109.5
O9—Cl2—O10111.9 (7)C2—C4A—H4A2109.5
O9—Cl2—O11110.0 (8)H4A1—C4A—H4A2109.5
O10—Cl2—O11110.3 (9)C2—C4A—H4A3109.5
O9—Cl2—O12109.5 (10)H4A1—C4A—H4A3109.5
O10—Cl2—O12107.3 (8)H4A2—C4A—H4A3109.5
O11—Cl2—O12107.7 (8)C2—C4B—H4B1109.5
C1—O1—Pt1127.4 (7)C2—C4B—H4B2109.5
C5—O2—Pt1127.9 (7)H4B1—C4B—H4B2109.5
O1—C1—O1i128.8 (12)C2—C4B—H4B3109.5
O1—C1—C2115.6 (6)H4B1—C4B—H4B3109.5
C3B—C2—C4B111.2 (12)H4B2—C4B—H4B3109.5
C4B—C2—C4Bi112 (2)C6—C7—H7A109.5
C3A—C2—C4A108.5 (11)C6—C7—H7B109.5
C4Ai—C2—C4A111.1 (18)H7A—C7—H7B109.5
C3B—C2—C1101.3 (15)C6—C7—H7C109.5
C4B—C2—C1110.2 (11)H7A—C7—H7C109.5
C3A—C2—C1106.8 (14)H7B—C7—H7C109.5
C4A—C2—C1110.9 (10)C6—C8—H8A109.5
O2—C5—O2i128.8 (12)C6—C8—H8B109.5
O2—C5—C6115.6 (6)H8A—C8—H8B109.5
C8—C6—C7111.5 (9)C6—C8—H8C109.5
C7—C6—C7i105.6 (14)H8A—C8—H8C109.5
C8—C6—C5107.5 (13)H8B—C8—H8C109.5
C7—C6—C5110.4 (8)C10—C11—H11A109.5
O4—C9—O3124.1 (18)C10—C11—H11B109.5
O4—C9—C10119.3 (17)H11A—C11—H11B109.5
O3—C9—C10116.6 (16)C10—C11—H11C109.5
C9—C10—C12106.3 (9)H11A—C11—H11C109.5
C12—C10—C12ii108.7 (13)H11B—C11—H11C109.5
C9—C10—C11113.9 (14)C10—C12—H12A109.5
C12—C10—C11110.6 (9)C10—C12—H12B109.5
Pt1—N1—H1A109.5H12A—C12—H12B109.5
Pt1—N1—H1B109.5C10—C12—H12C109.5
H1A—N1—H1B109.5H12A—C12—H12C109.5
Pt1—N1—H1C109.5H12B—C12—H12C109.5
O1—C1—C2—C3Bi90.0 (9)O1—C1—C2—C4A28.0 (15)
O1i—C1—C2—C3Bi90.0 (9)O1i—C1—C2—C4A152.0 (12)
O1—C1—C2—C3B90.0 (9)O2—C5—C6—C888.7 (10)
O1i—C1—C2—C3B90.0 (9)O2i—C5—C6—C888.7 (10)
O1—C1—C2—C4B27.8 (16)O2—C5—C6—C733.1 (16)
O1i—C1—C2—C4B152.2 (13)O2i—C5—C6—C7149.4 (11)
O1—C1—C2—C4Bi152.2 (13)O2—C5—C6—C7i149.4 (11)
O1i—C1—C2—C4Bi27.8 (16)O2i—C5—C6—C7i33.1 (16)
O1—C1—C2—C3A90.0 (9)O4—C9—C10—C12122.1 (9)
O1i—C1—C2—C3A90.0 (9)O3—C9—C10—C1257.9 (9)
O1—C1—C2—C4Ai152.0 (12)O4—C9—C10—C12ii122.1 (9)
O1i—C1—C2—C4Ai28.0 (15)O3—C9—C10—C12ii57.9 (9)
Symmetry codes: (i) x, y, z; (ii) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1C···O40.892.603.304 (10)136
N2—H2C···O80.892.933.244 (14)102
N2—H2B···O90.892.543.15 (2)126
N2—H2C···O5ii0.892.273.030 (15)145
N2—H2B···O9i0.892.693.30 (2)127
N2—H2B···O11i0.892.383.255 (16)168
N1—H1C···O10iii0.892.553.172 (14)128
N1—H1A···O6iv0.892.433.204 (19)146
N1—H1A···O12iv0.892.643.147 (16)117
N1—H1A···O6v0.892.243.043 (17)149
Symmetry codes: (i) x, y, z; (ii) x, y+1, z; (iii) x+1/2, y+1/2, z; (iv) x+1/2, y+1/2, z; (v) x+1/2, y1/2, z.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds