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In the title compound, [PtIII2Cl2(C4H6NO)2(NH3)4](SO4)·2H2O, the intradimer PtIII—PtIII distance is 2.6235 (13) Å. The axial PtIII—Cl bond distances for the N4 and N2O2 coordinated sites are 2.410 (5) and 2.446 (5) Å, respectively. The two Pt coordination planes are inclined at 16.3 (6)° and the average torsional twist of the ligands about the Pt–Pt axis is estimated as 0.4°.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804002065/cf6324sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804002065/cf6324Isup2.hkl
Contains datablock I

CCDC reference: 236016

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.035 Å
  • H-atom completeness 86%
  • Disorder in solvent or counterion
  • R factor = 0.059
  • wR factor = 0.153
  • Data-to-parameter ratio = 16.8

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT430_ALERT_2_A Short Inter D...A Contact O7B .. O8B = 2.24 Ang.
Author Response: They both have an occupation factor of 50 %, so the close contact between these two atoms could be avoided in a certain model.

Alert level B ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR) is > 1.50 Tmin and Tmax reported: 0.341 0.818 Tmin and Tmax expected: 0.184 0.818 RR = 1.849 Please check that your absorption correction is appropriate. PLAT060_ALERT_3_B Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.83 PLAT213_ALERT_2_B Atom C6 has ADP max/min Ratio ............. 4.10 oblate PLAT342_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 35
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.84 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C7 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... S1 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 46.00 Perc. PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C6 - C7 = 1.43 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl1 .. O8A = 3.22 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl1 .. O8B = 3.25 Ang. PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 O4 S PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 O2 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 O2
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:C8 H28 Cl2 N6 O8 Pt2 S1 Atom count from the _atom_site data: C8 H24 Cl2 N6 O8 Pt2 S1 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 C8 H28 Cl2 N6 O8 Pt2 S TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 16.00 16.00 0.00 H 56.00 48.00 8.00 Cl 4.00 4.00 0.00 N 12.00 12.00 0.00 O 16.00 16.00 0.00 Pt 4.00 4.00 0.00 S 2.00 2.00 0.00
1 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 13 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 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 5 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, TEXSAN (Molecular Structure Corporation, 2001), KENX and ORTEPII (Johnson, 1976).

Di-µ-α-pyrrolidinonato-bis[cis-diamminechloroplatinum(III)] sulfate dihydrate top
Crystal data top
[Pt2Cl2(C4H6NO)2(NH3)4](SO4)·2H2OZ = 2
Mr = 829.50F(000) = 776
Triclinic, P1? # Insert any comments here.
Hall symbol: -P 1Dx = 2.561 Mg m3
a = 8.906 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.865 (5) ÅCell parameters from 845 reflections
c = 13.619 (7) Åθ = 2.3–27.2°
α = 88.908 (9)°µ = 13.38 mm1
β = 78.705 (9)°T = 296 K
γ = 66.753 (9)°Plate, orange
V = 1075.7 (9) Å30.21 × 0.11 × 0.02 mm
Data collection top
Bruker SMART APEX CCD-detector
diffractometer
3904 independent reflections
Radiation source: fine-focus sealed tube2753 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.058
Detector resolution: 8.366 pixels mm-1θmax = 25.4°, θmin = 2.3°
ω scansh = 1010
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 1111
Tmin = 0.341, Tmax = 0.818l = 1616
8204 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)] = 0.059Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.153H-atom parameters constrained
S = 0.97 w = 1/[σ2(Fo2) + (0.0927P)2]
where P = (Fo2 + 2Fc2)/3
3904 reflections(Δ/σ)max < 0.001
233 parametersΔρmax = 5.39 e Å3
38 restraintsΔρmin = 1.90 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)

6.9037 (0.0284) x - 0.2804 (0.0494) y + 9.2632 (0.0498) z = 2.7078 (0.0191)

* -0.0024 (0.0064) N1 * 0.0024 (0.0064) N2 * 0.0023 (0.0064) N5 * -0.0023 (0.0064) N6 0.0178 (0.0066) Pt2 2.6084 (0.0073) Pt1

Rms deviation of fitted atoms = 0.0024

7.9064 (0.0193) x - 0.0043 (0.0452) y + 6.1215 (0.0561) z = 4.7508 (0.0197)

Angle to previous plane (with approximate e.s.d.) = 16.29 (0.59)

* 0.0085 (0.0058) O1 * -0.0085 (0.0058) O2 * -0.0083 (0.0056) N3 * 0.0082 (0.0056) N4 - 0.0766 (0.0058) Pt1 - 2.6793 (0.0061) Pt2

Rms deviation of fitted atoms = 0.0084

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)
Pt10.33988 (7)0.13501 (6)0.32469 (4)0.0324 (2)
Pt20.06810 (7)0.23551 (6)0.25062 (4)0.0336 (2)
Cl10.6124 (6)0.0341 (7)0.3721 (4)0.0659 (14)
Cl20.1696 (7)0.3266 (6)0.1714 (4)0.0687 (14)
S10.1244 (6)0.2888 (4)0.6173 (3)0.0483 (11)
O10.4382 (15)0.0211 (14)0.2115 (9)0.051 (3)
O20.4150 (15)0.2724 (14)0.2389 (8)0.051 (3)
O3A0.204 (3)0.217 (3)0.6908 (15)0.074 (3)*0.50
O3B0.143 (3)0.204 (2)0.7033 (14)0.074 (3)*0.50
O4A0.046 (3)0.194 (3)0.5244 (13)0.074 (3)*0.50
O4B0.2903 (17)0.376 (2)0.5950 (18)0.074 (3)*0.50
O5A0.007 (2)0.314 (2)0.6554 (17)0.074 (3)*0.50
O5B0.022 (3)0.187 (3)0.5299 (14)0.074 (3)*0.50
O6A0.245 (2)0.4307 (15)0.5956 (18)0.074 (3)*0.50
O6B0.049 (3)0.389 (2)0.6348 (18)0.074 (3)*0.50
O7A0.568 (7)0.342 (6)0.397 (4)0.132 (11)*0.50
O7B0.612 (6)0.316 (6)0.354 (4)0.132 (11)*0.50
O8A0.851 (8)0.170 (6)0.175 (5)0.191 (18)*0.50
O8B0.766 (8)0.261 (7)0.221 (5)0.191 (18)*0.50
N10.1991 (18)0.0696 (16)0.1458 (10)0.044 (3)
N20.1758 (18)0.3646 (15)0.1726 (10)0.048 (4)
N30.2803 (16)0.0118 (14)0.4127 (9)0.038 (3)
H3A0.36270.05990.44450.057*
H3B0.26530.07600.37490.057*
H3C0.18670.03620.45760.057*
N40.2596 (17)0.2899 (14)0.4424 (10)0.043 (3)
H4A0.33130.26160.48350.064*
H4B0.15930.29870.47570.064*
H4C0.25320.37650.41920.064*
N50.0443 (16)0.1077 (14)0.3288 (10)0.041 (3)
H5A0.14330.12910.31320.062*
H5B0.05800.12630.39440.062*
H5C0.01990.01250.31260.062*
N60.0689 (16)0.4053 (13)0.3557 (10)0.040 (3)
H6A0.16870.45520.34100.060*
H6B0.01640.46550.35630.060*
H6C0.08170.36950.41580.060*
C10.353 (2)0.0246 (19)0.1460 (12)0.045 (4)
C20.421 (3)0.148 (2)0.0651 (16)0.069 (6)
H2A0.42880.24160.09240.082*
H2B0.53020.15900.02720.082*
C30.287 (3)0.091 (3)0.0014 (14)0.076 (7)
H3D0.32900.05450.06010.092*
H3E0.25570.16950.01590.092*
C40.142 (3)0.030 (2)0.0618 (16)0.076 (7)
H4D0.10070.11430.02190.091*
H4E0.05240.00260.08600.091*
C50.319 (2)0.3591 (17)0.1872 (13)0.043 (4)
C60.369 (3)0.477 (2)0.1300 (16)0.073 (7)
H6D0.38380.54340.17490.088*
H6E0.46910.43210.07850.088*
C70.225 (3)0.550 (3)0.0878 (19)0.092 (8)
H7A0.26020.55870.01680.110*
H7B0.16350.64860.11960.110*
C80.109 (3)0.466 (3)0.1012 (19)0.084 (7)
H8A0.00670.53190.12710.101*
H8B0.11640.41570.03880.101*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.0366 (4)0.0403 (4)0.0291 (4)0.0274 (3)0.0007 (3)0.0004 (3)
Pt20.0463 (4)0.0367 (4)0.0275 (4)0.0265 (3)0.0076 (3)0.0026 (3)
Cl10.040 (2)0.104 (4)0.059 (3)0.034 (3)0.010 (2)0.002 (3)
Cl20.069 (3)0.087 (4)0.061 (3)0.034 (3)0.032 (3)0.013 (3)
S10.062 (3)0.034 (2)0.047 (3)0.029 (2)0.014 (2)0.0048 (18)
O10.052 (7)0.065 (8)0.042 (7)0.030 (6)0.008 (6)0.008 (6)
O20.065 (8)0.073 (8)0.037 (7)0.050 (7)0.012 (6)0.013 (6)
N10.062 (10)0.059 (9)0.031 (8)0.046 (8)0.005 (7)0.008 (6)
N20.060 (10)0.052 (9)0.029 (8)0.029 (8)0.012 (7)0.002 (7)
N30.040 (7)0.051 (8)0.030 (7)0.021 (6)0.016 (6)0.002 (6)
N40.051 (8)0.048 (8)0.038 (8)0.026 (7)0.014 (7)0.000 (6)
N50.043 (8)0.052 (8)0.039 (8)0.033 (7)0.004 (6)0.007 (6)
N60.041 (8)0.037 (7)0.048 (9)0.019 (6)0.013 (6)0.005 (6)
C10.067 (12)0.051 (10)0.036 (9)0.045 (10)0.005 (9)0.001 (8)
C20.084 (15)0.061 (12)0.064 (13)0.041 (11)0.008 (11)0.038 (10)
C30.116 (19)0.094 (16)0.033 (11)0.059 (15)0.006 (12)0.022 (11)
C40.082 (16)0.079 (15)0.072 (15)0.030 (13)0.034 (13)0.026 (12)
C50.064 (12)0.033 (8)0.039 (10)0.033 (8)0.006 (9)0.001 (7)
C60.096 (17)0.071 (14)0.065 (14)0.066 (13)0.024 (12)0.012 (11)
C70.11 (2)0.12 (2)0.075 (18)0.058 (18)0.042 (16)0.039 (16)
C80.097 (18)0.103 (18)0.085 (17)0.068 (16)0.037 (14)0.050 (15)
Geometric parameters (Å, º) top
Pt1—O12.003 (12)C5—C61.55 (2)
Pt1—O22.000 (11)C6—C71.42 (3)
Pt2—N12.002 (14)C7—C81.54 (3)
Pt2—N22.045 (12)N3—H3A0.890
Pt1—N32.027 (12)N3—H3B0.890
Pt1—N42.049 (13)N3—H3C0.890
Pt2—N52.062 (11)N4—H4A0.890
Pt2—N62.034 (13)N4—H4B0.890
Pt1—Cl12.446 (5)N4—H4C0.890
Pt2—Cl22.410 (5)N5—H5A0.890
Pt1—Pt22.6235 (13)N5—H5B0.890
S1—O6B1.448 (9)N5—H5C0.890
S1—O3A1.449 (9)N6—H6A0.890
S1—O3B1.450 (9)N6—H6B0.890
S1—O6A1.456 (9)N6—H6C0.890
S1—O4A1.464 (9)C2—H2A0.970
S1—O5B1.465 (9)C2—H2B0.970
S1—O5A1.473 (9)C3—H3D0.970
S1—O4B1.475 (9)C3—H3E0.970
O1—C11.289 (19)C4—H4D0.970
O2—C51.26 (2)C4—H4E0.970
N1—C11.32 (2)C6—H6D0.970
N1—C41.46 (2)C6—H6E0.970
N2—C51.31 (2)C7—H7A0.970
N2—C81.42 (2)C7—H7B0.970
C1—C21.51 (2)C8—H8A0.970
C2—C31.54 (3)C8—H8B0.970
C3—C41.47 (3)
O2—Pt1—O190.6 (5)H4A—N4—H4B109.5
O2—Pt1—N3176.0 (5)Pt1—N4—H4C109.5
O1—Pt1—N388.4 (5)H4A—N4—H4C109.5
O2—Pt1—N488.3 (5)H4B—N4—H4C109.5
O1—Pt1—N4175.1 (5)Pt2—N5—H5A109.5
N3—Pt1—N492.3 (5)Pt2—N5—H5B109.5
O2—Pt1—Cl188.5 (4)H5A—N5—H5B109.5
O1—Pt1—Cl187.3 (4)Pt2—N5—H5C109.5
N3—Pt1—Cl187.6 (4)H5A—N5—H5C109.5
N4—Pt1—Cl187.9 (4)H5B—N5—H5C109.5
O2—Pt1—Pt287.3 (3)Pt2—N6—H6A109.5
O1—Pt1—Pt286.9 (3)Pt2—N6—H6B109.5
N3—Pt1—Pt296.5 (3)H6A—N6—H6B109.5
N4—Pt1—Pt297.8 (4)Pt2—N6—H6C109.5
Cl1—Pt1—Pt2172.86 (13)H6A—N6—H6C109.5
N1—Pt2—N6178.9 (5)H6B—N6—H6C109.5
N1—Pt2—N289.9 (5)O1—C1—N1125.1 (15)
N6—Pt2—N290.2 (5)O1—C1—C2120.8 (17)
N1—Pt2—N590.5 (5)N1—C1—C2114.0 (16)
N6—Pt2—N589.4 (5)C1—C2—C3100.1 (16)
N2—Pt2—N5179.1 (5)C1—C2—H2A111.7
N1—Pt2—Cl293.1 (4)C3—C2—H2A111.7
N6—Pt2—Cl285.7 (4)C1—C2—H2B111.7
N2—Pt2—Cl293.1 (4)C3—C2—H2B111.7
N5—Pt2—Cl286.0 (4)H2A—C2—H2B109.5
N1—Pt2—Pt184.1 (4)C4—C3—C2107.3 (15)
N6—Pt2—Pt197.0 (4)C4—C3—H3D110.2
N2—Pt2—Pt184.0 (4)C2—C3—H3D110.2
N5—Pt2—Pt196.9 (4)C4—C3—H3E110.2
Cl2—Pt2—Pt1176.06 (14)C2—C3—H3E110.2
O6B—S1—O3B112.3 (9)H3D—C3—H3E108.5
O3A—S1—O6A111.2 (9)N1—C4—C3106.5 (17)
O3A—S1—O4A109.9 (9)N1—C4—H4D110.4
O6A—S1—O4A109.3 (9)C3—C4—H4D110.4
O6B—S1—O5B109.7 (9)N1—C4—H4E110.4
O3B—S1—O5B109.2 (9)C3—C4—H4E110.4
O3A—S1—O5A110.0 (9)H4D—C4—H4E108.6
O6A—S1—O5A108.4 (9)O2—C5—N2128.7 (14)
O4A—S1—O5A108.1 (9)O2—C5—C6119.6 (16)
O6B—S1—O4B108.5 (9)N2—C5—C6111.7 (16)
O3B—S1—O4B109.0 (9)C7—C6—C599.9 (17)
O5B—S1—O4B108.0 (9)C7—C6—H6D111.8
C1—O1—Pt1120.6 (11)C5—C6—H6D111.8
C5—O2—Pt1119.5 (10)C7—C6—H6E111.8
C1—N1—C4109.8 (15)C5—C6—H6E111.8
C1—N1—Pt2123.2 (11)H6D—C6—H6E109.5
C4—N1—Pt2127.0 (13)C6—C7—C8112.3 (19)
C5—N2—C8113.9 (15)C6—C7—H7A109.1
C5—N2—Pt2120.1 (11)C8—C7—H7A109.1
C8—N2—Pt2126.0 (13)C6—C7—H7B109.1
Pt1—N3—H3A109.5C8—C7—H7B109.1
Pt1—N3—H3B109.5H7A—C7—H7B107.9
H3A—N3—H3B109.5N2—C8—C7100.6 (17)
Pt1—N3—H3C109.5N2—C8—H8A111.7
H3A—N3—H3C109.5C7—C8—H8A111.7
H3B—N3—H3C109.5N2—C8—H8B111.7
Pt1—N4—H4A109.5C7—C8—H8B111.7
Pt1—N4—H4B109.5H8A—C8—H8B109.4
O1—Pt1—Pt2—N10.6 (5)C1—N1—C4—C37 (2)
N4—Pt1—Pt2—N61.9 (5)C2—C3—C4—N114 (2)
O2—Pt1—Pt2—N20.3 (5)C8—N2—C5—O2173.5 (19)
N3—Pt1—Pt2—N51.1 (5)C8—N2—C5—C66 (2)
C4—N1—C1—O1179.0 (16)O2—C5—C6—C7177.7 (19)
C4—N1—C1—C23 (2)N2—C5—C6—C73 (2)
O1—C1—C2—C3172.8 (16)C5—C6—C7—C810 (3)
N1—C1—C2—C311 (2)C5—N2—C8—C711 (3)
C1—C2—C3—C414 (2)C6—C7—C8—N213 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N3—H3A···Cl1i0.892.583.233 (13)131
N3—H3C···O4A0.892.082.93 (2)161
N3—H3C···O5B0.891.952.82 (2)163
N3—H3B···O3Aii0.891.972.85 (3)171
N3—H3B···O3Bii0.892.343.20 (3)163
N4—H4B···O4A0.892.413.21 (3)150
N4—H4B···O5A0.892.533.25 (3)139
N4—H4B···O5B0.892.303.09 (3)148
N4—H4B···O6B0.892.473.24 (3)145
N4—H4C···O4Biii0.892.593.44 (3)159
N4—H4C···O6Aiii0.891.882.75 (2)165
N4—H4C···O6Biii0.892.523.26 (3)141
N5—H5B···O4A0.891.942.81 (2)164
N5—H5B···O5B0.892.072.93 (2)161
N5—H5C···O3Aii0.892.203.07 (3)164
N5—H5C···O3Bii0.891.972.85 (3)171
N6—H6C···O4A0.892.223.05 (3)156
N6—H6C···O5B0.892.323.15 (3)155
N6—H6C···O6A0.892.543.30 (3)145
N6—H6B···O5Aiii0.892.213.02 (2)152
N6—H6B···O6Biii0.891.762.637 (16)169
N3—H3B···O3Aii0.891.972.85 (3)171
N3—H3B···O3Bii0.892.343.20 (3)163
N5—H5C···O3Bii0.891.972.85 (3)171
N5—H5C···O3Bii0.891.972.85 (3)171
N4—H4C···O6Aiii0.891.882.75 (2)165
N6—H6B···O5Aiii0.892.213.02 (2)152
N6—H6B···O6Biii0.891.762.637 (16)169
N4—H4A···O7Ai0.892.293.06 (6)145
N4—H4A···O7Bi0.892.483.25 (5)146
Symmetry codes: (i) x+1, y, z+1; (ii) x, y, z+1; (iii) x, y+1, z+1.
 

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