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In the title compound, [PtII2(C4H6NO)2(NH3)4](SO4)·H2O, the intradimer PtII—PtII distance is 2.9749 (11) Å, which is clearly shorter than the value of 3.029 (2) Å reported for a different salt of the same cation, viz. [PtII2(C4H6NO)2(NH3)4]2(PF6)3(NO3)·H2O [Matsumoto et al. (1989). Inorg. Chem. 28, 2959–2964]. The two Pt coordination planes are inclined to each other by 29.9 (5)°, and the average torsional twist of the ligands about the Pt—Pt axis is estimated as 4.3 (8)°.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804002442/lh6164sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804002442/lh6164Isup2.hkl
Contains datablock I

CCDC reference: 236022

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.028 Å
  • H-atom completeness 93%
  • R factor = 0.054
  • wR factor = 0.126
  • Data-to-parameter ratio = 13.6

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.93
Author Response: We have tried to cut of the higher angle region of the present reflection data to solve this problem. However, we have been unsuccessful in solving this problem thus far.
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......         O7
Author Response: It is generally hard to locate the H atoms of water molecules in the X-ray structure determination of platinum complexes. Some suggest that H atoms of water molecules should be located based on the method of Nardelli. However, we usually do not locate them, since we believe that crystallography is the method to extract the positions of atoms from the experimental data and we therefore do not want to rely on the mere calculations.

Alert level B PLAT342_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 28 PLAT430_ALERT_2_B Short Inter D...A Contact O5 .. O7 = 2.82 Ang.
Alert level C REFLT03_ALERT_3_C Reflection count < 95% complete From the CIF: _diffrn_reflns_theta_max 68.24 From the CIF: _diffrn_reflns_theta_full 0.00 From the CIF: _reflns_number_total 3014 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 3247 Completeness (_total/calc) 92.82% PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.93 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)... ? PLAT213_ALERT_2_C Atom N5 has ADP max/min Ratio ............. 3.20 oblate 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 PLAT420_ALERT_2_C D-H Without Acceptor N3 - H3C ... ? PLAT430_ALERT_2_C Short Inter D...A Contact O3 .. O7 = 2.88 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 O
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 H26 N6 O7 Pt2 S1 Atom count from the _atom_site data: C8 H24 N6 O7 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 H26 N6 O7 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 52.00 48.00 4.00 N 12.00 12.00 0.00 O 14.00 14.00 0.00 Pt 4.00 4.00 0.00 S 2.00 2.00 0.00
2 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 12 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 7 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 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; 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-diammineplatinum(II)] sulfate hydrate top
Crystal data top
[Pt2(C4H6NO)2(NH3)4](SO4)·H2OZ = 2
Mr = 740.59F(000) = 688
Triclinic, P1Dx = 2.777 Mg m3
Hall symbol: -P 1Cu Kα radiation, λ = 1.54180 Å
a = 6.859 (2) ÅCell parameters from 1567 reflections
b = 10.229 (2) Åθ = 5.1–68.2°
c = 12.896 (2) ŵ = 30.63 mm1
α = 99.569 (10)°T = 293 K
β = 93.538 (10)°Needle, colorless
γ = 95.146 (10)°0.13 × 0.05 × 0.03 mm
V = 885.8 (3) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
3014 independent reflections
Radiation source: fine-focus sealed tube2176 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.072
ω scansθmax = 68.2°, θmin = 5.1°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 77
Tmin = 0.098, Tmax = 0.465k = 1212
3014 measured reflectionsl = 1515
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.054H-atom parameters constrained
wR(F2) = 0.127 w = 1/[σ2(Fo2) + (0.0513P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max < 0.001
3014 reflectionsΔρmax = 2.52 e Å3
222 parametersΔρmin = 2.15 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00037 (8)
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)

6.4829 (0.0115) x - 1.3311 (0.0493) y - 4.7492 (0.0590) z = 1.5729 (0.0194)

* 0.0085 (0.0063) O1 * -0.0087 (0.0064) O2 * -0.0089 (0.0066) N3 * 0.0091 (0.0067) N4 - 0.0936 (0.0065) Pt1 - 2.9362 (0.0072) Pt2

Rms deviation of fitted atoms = 0.0088

-4.5054 (0.0267) x + 1.2023 (0.0500) y + 9.9212 (0.0417) z = 2.6877 (0.0184)

Angle to previous plane (with approximate e.s.d.) = 29.94 (1/2)

* -0.0013 (0.0069) N1 * 0.0013 (0.0068) N2 * 0.0013 (0.0068) N5 * -0.0012 (0.0067) N6 0.0217 (0.0068) Pt2 - 2.8781 (0.0078) Pt1

Rms deviation of fitted atoms = 0.0013

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
Pt10.36898 (10)0.27545 (7)0.11499 (5)0.0357 (2)
Pt20.04202 (10)0.32841 (6)0.25238 (5)0.0320 (2)
S10.2172 (6)0.2402 (4)0.1152 (3)0.0352 (9)
O10.4881 (18)0.4458 (12)0.2083 (9)0.047 (3)
O20.4409 (17)0.1671 (12)0.2256 (10)0.048 (3)
O30.422 (2)0.2011 (19)0.1427 (13)0.090 (6)
O40.136 (2)0.1445 (13)0.0575 (11)0.066 (4)
O50.108 (2)0.2489 (13)0.2066 (11)0.062 (4)
O60.197 (3)0.3696 (13)0.0458 (11)0.081 (5)
O70.202 (2)0.0886 (14)0.2468 (12)0.065 (4)
N10.238 (2)0.4775 (13)0.3212 (10)0.037 (3)
N20.174 (2)0.2013 (14)0.3256 (11)0.039 (3)
N30.315 (2)0.3740 (12)0.0046 (11)0.042 (3)
H3A0.40710.36240.04980.062*
H3B0.31500.46050.02070.062*
H3C0.19780.34270.03760.062*
N40.277 (2)0.1081 (14)0.0149 (11)0.048 (4)
H4A0.36610.09100.03170.072*
H4B0.16350.11760.01890.072*
H4C0.26070.04090.05040.072*
N50.0889 (17)0.4588 (14)0.1751 (11)0.037 (3)
H5A0.00360.52920.17350.056*
H5B0.19210.48510.20840.056*
H5C0.12830.41910.10940.056*
N60.1564 (19)0.1773 (14)0.1783 (12)0.042 (3)
H6A0.13530.15940.11020.063*
H6B0.27720.20120.18490.063*
H6C0.14360.10510.20720.063*
C10.413 (2)0.5057 (16)0.2883 (13)0.038 (4)
C20.522 (3)0.6238 (18)0.3557 (15)0.058 (6)
H2A0.54830.69520.31600.069*
H2B0.64550.60170.38580.069*
C30.384 (3)0.663 (2)0.4410 (17)0.072 (6)
H3D0.44410.65420.50940.086*
H3E0.35660.75430.44310.086*
C40.198 (3)0.571 (2)0.4151 (16)0.061 (6)
H4D0.17020.52420.47300.073*
H4E0.08810.61970.40010.073*
C50.331 (2)0.1455 (16)0.2985 (13)0.036 (4)
C60.389 (3)0.0468 (16)0.3669 (13)0.043 (4)
H6D0.51440.07580.40640.052*
H6E0.39270.04130.32580.052*
C70.217 (3)0.051 (2)0.4399 (15)0.065 (6)
H7A0.14420.03680.43040.078*
H7B0.26900.07420.51300.078*
C80.084 (3)0.1494 (18)0.4150 (13)0.043 (4)
H8A0.08110.22020.47490.052*
H8B0.04790.10770.39420.052*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.0335 (5)0.0343 (4)0.0410 (4)0.0056 (3)0.0039 (3)0.0096 (3)
Pt20.0297 (5)0.0340 (4)0.0342 (4)0.0050 (3)0.0005 (3)0.0112 (3)
S10.039 (3)0.034 (2)0.0329 (18)0.0071 (17)0.0009 (17)0.0064 (15)
O10.043 (8)0.046 (7)0.050 (7)0.007 (6)0.000 (6)0.003 (6)
O20.045 (8)0.054 (8)0.051 (7)0.019 (6)0.009 (6)0.025 (6)
O30.035 (9)0.146 (16)0.077 (11)0.001 (9)0.006 (8)0.010 (10)
O40.095 (12)0.050 (8)0.060 (8)0.017 (8)0.000 (8)0.027 (7)
O50.078 (10)0.053 (8)0.063 (8)0.026 (7)0.023 (8)0.022 (7)
O60.140 (15)0.039 (8)0.061 (9)0.008 (9)0.002 (10)0.001 (7)
O70.055 (9)0.061 (9)0.077 (10)0.011 (7)0.014 (7)0.002 (7)
N10.032 (9)0.042 (8)0.037 (7)0.005 (6)0.003 (6)0.007 (6)
N20.030 (9)0.043 (8)0.044 (8)0.009 (6)0.001 (6)0.003 (6)
N30.056 (10)0.026 (7)0.045 (8)0.011 (6)0.010 (7)0.006 (6)
N40.065 (11)0.045 (9)0.038 (7)0.007 (7)0.002 (7)0.017 (6)
N50.009 (7)0.061 (9)0.049 (8)0.010 (6)0.000 (6)0.024 (7)
N60.023 (8)0.051 (9)0.056 (9)0.003 (6)0.002 (6)0.020 (7)
C10.023 (10)0.043 (10)0.046 (9)0.000 (7)0.016 (8)0.011 (8)
C20.068 (15)0.041 (10)0.053 (11)0.027 (9)0.017 (10)0.001 (9)
C30.083 (17)0.063 (14)0.058 (12)0.004 (12)0.003 (12)0.014 (11)
C40.072 (15)0.051 (12)0.062 (12)0.029 (11)0.014 (11)0.004 (10)
C50.026 (10)0.035 (9)0.048 (9)0.005 (7)0.009 (8)0.012 (7)
C60.059 (13)0.030 (9)0.041 (9)0.013 (8)0.015 (8)0.008 (7)
C70.075 (15)0.090 (16)0.045 (10)0.016 (12)0.021 (10)0.049 (11)
C80.043 (11)0.055 (11)0.038 (9)0.013 (9)0.012 (8)0.017 (8)
Geometric parameters (Å, º) top
Pt1—N41.991 (14)C7—C81.48 (2)
Pt1—O22.011 (11)N3—H3A0.8900
Pt1—N32.012 (12)N3—H3B0.8900
Pt1—O12.020 (12)N3—H3C0.8900
Pt2—N21.978 (13)N4—H4A0.8900
Pt2—N11.990 (14)N4—H4B0.8900
Pt2—N52.030 (11)N4—H4C0.8900
Pt2—N62.031 (14)N5—H5A0.8900
Pt1—Pt22.9749 (11)N5—H5B0.8900
Pt1—Pt2i4.7921 (16)N5—H5C0.8900
S1—O31.431 (15)N6—H6A0.8900
S1—O51.444 (14)N6—H6B0.8900
S1—O41.453 (12)N6—H6C0.8900
S1—O61.460 (14)C2—H2A0.9700
O1—C11.27 (2)C2—H2B0.9700
O2—C51.28 (2)C3—H3D0.9700
N1—C11.32 (2)C3—H3E0.9700
N1—C41.47 (2)C4—H4D0.9700
N2—C51.30 (2)C4—H4E0.9700
N2—C81.49 (2)C6—H6D0.9700
C1—C21.48 (2)C6—H6E0.9700
C2—C31.52 (3)C7—H7A0.9700
C3—C41.50 (3)C7—H7B0.9700
C5—C61.510 (19)C8—H8A0.9700
C6—C71.55 (3)C8—H8B0.9700
O5···O72.820 (18)O7···O3i2.88 (2)
N4—Pt1—O289.7 (5)H5A—N5—H5C109.5
N4—Pt1—N387.3 (5)H5B—N5—H5C109.5
O2—Pt1—N3174.4 (5)Pt2—N6—H6A109.5
N4—Pt1—O1174.0 (5)Pt2—N6—H6B109.5
O2—Pt1—O191.5 (5)H6A—N6—H6B109.5
N3—Pt1—O191.0 (5)Pt2—N6—H6C109.5
N2—Pt2—N191.0 (5)H6A—N6—H6C109.5
N2—Pt2—N5178.8 (5)H6B—N6—H6C109.5
N1—Pt2—N588.7 (5)O1—C1—N1127.8 (15)
N2—Pt2—N689.8 (5)O1—C1—C2120.2 (16)
N1—Pt2—N6178.4 (5)N1—C1—C2112.0 (16)
N5—Pt2—N690.4 (5)C1—C2—C3103.4 (16)
N4—Pt1—Pt2105.7 (4)C1—C2—H2A111.1
O2—Pt1—Pt281.2 (3)C3—C2—H2A111.1
N3—Pt1—Pt2104.1 (4)C1—C2—H2B111.1
O1—Pt1—Pt280.3 (4)C3—C2—H2B111.1
N2—Pt2—Pt179.9 (4)H2A—C2—H2B109.0
N1—Pt2—Pt180.9 (4)C4—C3—C2107.7 (16)
N5—Pt2—Pt198.9 (4)C4—C3—H3D110.2
N6—Pt2—Pt197.9 (4)C2—C3—H3D110.2
O3—S1—O5112.5 (9)C4—C3—H3E110.2
O3—S1—O4109.3 (10)C2—C3—H3E110.2
O5—S1—O4109.0 (8)H3D—C3—H3E108.5
O3—S1—O6108.2 (10)N1—C4—C3104.0 (16)
O5—S1—O6109.6 (9)N1—C4—H4D111.0
O4—S1—O6108.1 (8)C3—C4—H4D111.0
C1—O1—Pt1125.3 (11)N1—C4—H4E111.0
C5—O2—Pt1123.3 (10)C3—C4—H4E111.0
C1—N1—C4112.8 (15)H4D—C4—H4E109.0
C1—N1—Pt2125.2 (11)O2—C5—N2128.5 (15)
C4—N1—Pt2122.0 (13)O2—C5—C6117.8 (15)
C5—N2—C8112.8 (13)N2—C5—C6113.7 (16)
C5—N2—Pt2126.4 (12)C5—C6—C7100.0 (13)
C8—N2—Pt2120.6 (10)C5—C6—H6D111.8
Pt1—N3—H3A109.5C7—C6—H6D111.8
Pt1—N3—H3B109.5C5—C6—H6E111.8
H3A—N3—H3B109.5C7—C6—H6E111.8
Pt1—N3—H3C109.5H6D—C6—H6E109.5
H3A—N3—H3C109.5C8—C7—C6110.1 (13)
H3B—N3—H3C109.5C8—C7—H7A109.6
Pt1—N4—H4A109.5C6—C7—H7A109.6
Pt1—N4—H4B109.5C8—C7—H7B109.6
H4A—N4—H4B109.5C6—C7—H7B109.6
Pt1—N4—H4C109.5H7A—C7—H7B108.1
H4A—N4—H4C109.5C7—C8—N2103.3 (13)
H4B—N4—H4C109.5C7—C8—H8A111.1
Pt2—N5—H5A109.5N2—C8—H8A111.1
Pt2—N5—H5B109.5C7—C8—H8B111.1
H5A—N5—H5B109.5N2—C8—H8B111.1
Pt2—N5—H5C109.5H8A—C8—H8B109.1
O2—Pt1—Pt2—N23.5 (5)C1—N1—C4—C33 (2)
O1—Pt1—Pt2—N13.9 (5)C2—C3—C4—N14 (2)
N3—Pt1—Pt2—N55.2 (6)C8—N2—C5—O2180.0 (16)
N4—Pt1—Pt2—N64.7 (5)C8—N2—C5—C63 (2)
C4—N1—C1—O1178.3 (16)O2—C5—C6—C7179.1 (16)
C4—N1—C1—C20 (2)N2—C5—C6—C73.2 (19)
O1—C1—C2—C3179.2 (16)C5—C6—C7—C83 (2)
N1—C1—C2—C32 (2)C6—C7—C8—N21 (2)
C1—C2—C3—C43 (2)C5—N2—C8—C71 (2)
Symmetry code: (i) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N4—H4B···O40.892.143.00 (2)164
N5—H5C···O60.892.002.87 (2)167
N6—H6A···O40.892.143.02 (2)167
N3—H3B···O6ii0.891.972.798 (18)154
N3—H3A···O3i0.892.323.08 (2)143
N4—H4C···O4iii0.892.032.829 (19)149
N4—H4A···O3i0.892.443.18 (2)141
N5—H5A···O5ii0.892.293.12 (2)155
N5—H5A···O6ii0.892.503.23 (2)140
N5—H5B···O1iv0.892.192.954 (17)143
N6—H6C···O7iii0.892.142.99 (2)161
N6—H6B···O2iv0.892.052.862 (18)151
Symmetry codes: (i) x+1, y, z; (ii) x, y+1, z; (iii) x, y, z; (iv) x1, y, z.
 

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