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The title compound, [Pt2(μ-C4H7O2)2(NH3)4]2(ClO4)4, involves two independent diplatinum(II) units. For each unit, a pair of dimeric units located around an inversion center are associated with one another to give a tetranuclear PtII4 cation, in which the interdimer association is stabilized by four hydrogen bonds formed between the ammines and the butyrate O atoms. The intradimer and interdimer Pt—Pt distances within these tetraplatinum(II) chain cations are, respectively, 2.9881 (4) and 3.2619 (6) Å for one set of dimers, and 3.0246 (4) and 3.3049 (6) Å for the other set of dimers.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680302782X/ob6329sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680302782X/ob6329Isup2.hkl
Contains datablock I

CCDC reference: 231821

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.015 Å
  • H-atom completeness 97%
  • Disorder in solvent or counterion
  • R factor = 0.043
  • wR factor = 0.102
  • Data-to-parameter ratio = 20.2

checkCIF/PLATON results

No syntax errors found



Alert level B ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR) is > 1.50 Tmin and Tmax reported: 0.205 0.536 Tmin and Tmax expected: 0.121 0.536 RR = 1.691 Please check that your absorption correction is appropriate. PLAT060_ALERT_3_B Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.66 PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors .... C10 PLAT326_ALERT_2_B Check for Possibly Missing H on sp3? Carbon .... C10
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)... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.80 Ratio PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C11A PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C11B PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C16A PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C16B PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C14 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C2 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C6 PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O17A PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O17B PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O18B PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O19A PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O20A PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O20B PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O21A PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O21B PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O22A PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O22B PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O23A PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O23B PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O24A PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O24B PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl3 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl4 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 ......................... 5.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 29.00 Perc. PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 15 PLAT480_ALERT_4_C Long H...A H-Bond Reported H5A .. O2 = 2.71 Ang.
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:C16 H52 Cl4 N8 O24 Pt4 Atom count from the _atom_site data: C16 H50 Cl4 N8 O24 Pt4 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 C16 H52 Cl4 N8 O24 Pt4 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 32.00 32.00 0.00 H 104.00 100.00 4.00 Cl 8.00 8.00 0.00 N 16.00 16.00 0.00 O 48.00 48.00 0.00 Pt 8.00 8.00 0.00
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 33 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 11 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 20 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).

Bis{di-µ-isobutyrato-bis[cis-diammineplatinum(II)]} tetrakis(perchlorate) top
Crystal data top
[Pt2(C4H7O2)2(NH3)4]2(ClO4)4Z = 2
Mr = 1662.82F(000) = 1552
Triclinic, P1Dx = 2.509 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.1557 (6) ÅCell parameters from 5928 reflections
b = 14.5963 (8) Åθ = 2.2–28.3°
c = 15.5209 (9) ŵ = 13.00 mm1
α = 74.354 (1)°T = 296 K
β = 84.621 (1)°Prism, yellow
γ = 85.052 (1)°0.31 × 0.14 × 0.05 mm
V = 2201.3 (2) Å3
Data collection top
Bruker SMART APEX CCD-detector
diffractometer
10024 independent reflections
Radiation source: fine-focus sealed tube7784 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.058
Detector resolution: 8.366 pixels mm-1θmax = 27.5°, θmin = 2.2°
ω scansh = 1313
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 1818
Tmin = 0.205, Tmax = 0.536l = 2020
21380 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)] = 0.043Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.102H-atom parameters constrained
S = 0.96 w = 1/[σ2(Fo2) + (0.0372P)2]
where P = (Fo2 + 2Fc2)/3
10024 reflections(Δ/σ)max < 0.001
497 parametersΔρmax = 2.97 e Å3
49 restraintsΔρmin = 2.16 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)

-2.2992 (0.0211) x + 13.8320 (0.0099) y + 2.4412 (0.0317) z = 6.5912 (0.0180)

* -0.0026 (0.0028) N1 * 0.0026 (0.0028) N2 * 0.0026 (0.0028) O1 * -0.0026 (0.0028) O3 - 0.0813 (0.0029) Pt1 - 2.9353 (0.0030) Pt2

Rms deviation of fitted atoms = 0.0026

-3.9774 (0.0204) x + 10.7045 (0.0218) y + 10.0759 (0.0257) z = 6.1949 (0.0140)

Angle to previous plane (with approximate e.s.d.) = 37.24 (0.18)

* 0.0125 (0.0030) N3 * -0.0127 (0.0030) N4 * -0.0124 (0.0030) O2 * 0.0126 (0.0030) O4 0.1024 (0.0030) Pt2 2.9081 (0.0032) Pt1

Rms deviation of fitted atoms = 0.0126

-3.0787 (0.0224) x + 13.1802 (0.0150) y + 6.2784 (0.0322) z = 2.5589 (0.0125)

Angle to previous plane (with approximate e.s.d.) = 20.69 (1/4)

* -0.0121 (0.0033) N5 * 0.0120 (0.0032) N6 * 0.0119 (0.0032) O5 * -0.0119 (0.0032) O7 - 0.0880 (0.0032) Pt3 - 2.9164 (0.0037) Pt4

Rms deviation of fitted atoms = 0.0120

-2.4050 (0.0237) x + 8.0743 (0.0289) y + 13.6666 (0.0180) z = 0.3493 (0.0126)

Angle to previous plane (with approximate e.s.d.) = 40.36 (0.22)

* 0.0138 (0.0032) N7 * -0.0139 (0.0033) N8 * -0.0137 (0.0032) O6 * 0.0139 (0.0033) O8 0.0841 (0.0033) Pt4 2.9313 (0.0035) Pt3

Rms deviation of fitted atoms = 0.0138

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)
Pt10.03826 (3)0.38756 (2)0.50681 (2)0.03241 (9)
Pt20.16675 (3)0.20936 (2)0.46839 (2)0.02939 (9)
Pt30.34062 (3)0.17275 (2)0.19793 (2)0.03620 (9)
Pt40.46568 (3)0.03829 (2)0.09104 (2)0.03489 (9)
Cl10.8086 (2)0.12558 (16)0.29275 (16)0.0472 (5)
Cl20.3480 (2)0.09795 (15)0.44009 (16)0.0439 (5)
Cl30.4254 (2)0.30054 (16)0.71422 (19)0.0571 (6)
Cl40.0307 (2)0.13471 (18)0.76021 (16)0.0509 (6)
O10.0156 (6)0.4071 (4)0.3798 (4)0.0413 (14)
O20.0737 (6)0.2711 (4)0.3547 (4)0.0430 (15)
O30.2212 (5)0.4328 (4)0.4552 (4)0.0407 (14)
O40.3154 (5)0.2981 (4)0.4239 (4)0.0390 (14)
O50.2335 (6)0.2077 (4)0.0879 (4)0.0521 (17)
O60.2998 (6)0.0918 (4)0.0231 (4)0.0469 (15)
O70.4934 (6)0.2474 (4)0.1282 (4)0.0513 (17)
O80.5598 (6)0.1591 (4)0.0311 (4)0.0443 (15)
O90.8830 (10)0.1513 (7)0.2094 (6)0.112 (3)
O100.8979 (7)0.0747 (6)0.3568 (5)0.077 (2)
O110.7075 (7)0.0637 (6)0.2909 (7)0.086 (3)
O120.7473 (8)0.2079 (5)0.3149 (6)0.091 (3)
O130.2622 (7)0.0176 (4)0.4497 (5)0.068 (2)
O140.2707 (7)0.1785 (5)0.4596 (6)0.076 (2)
O150.4471 (7)0.1144 (6)0.5015 (6)0.079 (2)
O160.4078 (8)0.0772 (5)0.3508 (5)0.076 (2)
O17A0.5632 (9)0.3129 (12)0.6867 (10)0.0924 (19)*0.50
O17B0.5628 (9)0.3072 (14)0.7117 (11)0.0924 (19)*0.50
O18A0.3704 (14)0.2595 (10)0.6529 (9)0.0924 (19)*0.50
O18B0.3866 (15)0.3167 (12)0.6238 (7)0.0924 (19)*0.50
O19A0.4141 (14)0.2374 (9)0.8016 (7)0.0924 (19)*0.50
O19B0.3904 (15)0.2071 (8)0.7615 (10)0.0924 (19)*0.50
O20A0.3591 (16)0.3897 (7)0.7125 (10)0.0924 (19)*0.50
O20B0.3573 (18)0.3747 (11)0.7474 (13)0.0924 (19)*0.50
O21A0.0929 (16)0.2304 (7)0.7569 (10)0.105 (2)*0.50
O21B0.079 (2)0.2141 (11)0.7944 (14)0.105 (2)*0.50
O22A0.0620 (15)0.0738 (9)0.8456 (7)0.105 (2)*0.50
O22B0.0962 (18)0.0528 (10)0.8099 (12)0.105 (2)*0.50
O23A0.1062 (9)0.1439 (11)0.7393 (11)0.105 (2)*0.50
O23B0.1056 (10)0.1094 (14)0.7748 (15)0.105 (2)*0.50
O24A0.0881 (15)0.1021 (11)0.6930 (9)0.105 (2)*0.50
O24B0.063 (2)0.1497 (14)0.6697 (8)0.105 (2)*0.50
N10.1493 (7)0.3533 (5)0.5563 (6)0.049 (2)
H1A0.20330.40580.54560.073*
H1B0.15000.32710.61520.073*
H1C0.17640.31210.52970.073*
N20.0911 (7)0.3805 (5)0.6310 (5)0.0404 (17)
H2A0.17910.37730.63060.061*
H2B0.05990.32880.66980.061*
H2C0.05760.43220.64720.061*
N30.0287 (7)0.1122 (5)0.5082 (5)0.0449 (18)
H3A0.02270.11700.46360.067*
H3B0.02060.12290.55540.067*
H3C0.06850.05400.52310.067*
N40.2709 (7)0.1395 (5)0.5723 (5)0.0445 (18)
H4A0.34410.16940.57120.067*
H4B0.29290.08030.56860.067*
H4C0.22210.13780.62330.067*
N50.1818 (7)0.1079 (5)0.2683 (5)0.0488 (19)
H5A0.10850.14470.25310.073*
H5B0.19010.09820.32670.073*
H5C0.17650.05220.25610.073*
N60.4369 (7)0.1494 (5)0.3100 (5)0.0424 (17)
H6A0.51850.16930.29570.064*
H6B0.44130.08740.33740.064*
H6C0.39360.18130.34660.064*
N70.3775 (7)0.0855 (5)0.1435 (5)0.0485 (19)
H7A0.41810.13040.11970.073*
H7B0.29270.07750.13130.073*
H7C0.38270.10310.20270.073*
N80.6372 (7)0.0185 (5)0.1476 (6)0.051 (2)
H8A0.62160.07210.18980.077*
H8B0.66860.02300.17200.077*
H8C0.69640.03110.10560.077*
C10.0139 (8)0.3505 (6)0.3309 (6)0.0383 (19)
C20.0205 (10)0.3828 (7)0.2338 (7)0.051 (2)
H20.03950.32590.21620.061*
C30.1389 (12)0.4510 (9)0.2177 (8)0.083 (4)
H3D0.11910.51070.22660.124*
H3E0.21160.42560.25890.124*
H3F0.16240.46060.15730.124*
C40.0993 (12)0.4233 (10)0.1768 (8)0.093 (4)
H4D0.12940.47260.19910.139*
H4E0.07670.44950.11600.139*
H4F0.16850.37370.17900.139*
C50.3154 (8)0.3832 (6)0.4236 (6)0.0380 (19)
C60.4371 (8)0.4357 (6)0.3796 (6)0.042 (2)
H60.42080.50230.38170.050*
C70.5544 (10)0.3950 (8)0.4313 (8)0.074 (3)
H7D0.57920.33230.42420.110*
H7E0.53270.39120.49360.110*
H7F0.62700.43510.40930.110*
C80.4589 (12)0.4350 (10)0.2848 (8)0.093 (5)
H8D0.53790.46660.25890.140*
H8E0.38450.46760.25300.140*
H8F0.46840.37030.28060.140*
C90.2261 (9)0.1618 (6)0.0313 (6)0.043 (2)
C100.1209 (9)0.1938 (7)0.0352 (7)0.050 (2)
C11A0.119 (3)0.303 (2)0.082 (2)0.094 (6)*0.50
H11A0.06890.31660.13390.141*0.50
H11B0.20840.32070.10010.141*0.50
H11C0.07940.33760.04110.141*0.50
C11B0.073 (3)0.298 (2)0.041 (2)0.094 (6)*0.50
H11D0.02110.32240.09160.141*0.50
H11E0.14860.33540.04760.141*0.50
H11F0.02040.30110.01300.141*0.50
C120.0007 (13)0.1478 (11)0.0083 (10)0.107 (5)
H12A0.01490.07980.02110.160*
H12B0.07110.16810.03110.160*
H12C0.02500.16550.06310.160*
C130.5579 (9)0.2330 (7)0.0590 (6)0.047 (2)
C140.6404 (13)0.3114 (8)0.0047 (8)0.076 (4)
C150.7024 (16)0.3597 (10)0.0598 (10)0.122 (6)
H15A0.76000.40550.02210.183*
H15B0.75300.31380.10270.183*
H15C0.63510.39180.09070.183*
C16A0.661 (3)0.325 (2)0.070 (2)0.114 (8)*0.50
H16A0.58520.35860.09930.171*0.50
H16B0.67800.26490.08480.171*0.50
H16C0.73670.36200.08910.171*0.50
C16B0.540 (3)0.380 (2)0.057 (2)0.114 (8)*0.50
H16D0.58570.41080.11310.171*0.50
H16E0.50100.42720.02810.171*0.50
H16F0.47160.34390.06820.171*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.03024 (17)0.02851 (16)0.0422 (2)0.00238 (12)0.00290 (13)0.01698 (14)
Pt20.03077 (16)0.02392 (15)0.03383 (19)0.00107 (11)0.00238 (12)0.01001 (13)
Pt30.03871 (19)0.03870 (19)0.03267 (19)0.00409 (13)0.00091 (13)0.01516 (15)
Pt40.03641 (18)0.03552 (18)0.03400 (19)0.00310 (13)0.00032 (13)0.01376 (15)
Cl10.0459 (13)0.0500 (13)0.0450 (14)0.0006 (10)0.0003 (10)0.0131 (11)
Cl20.0381 (12)0.0408 (12)0.0532 (14)0.0000 (9)0.0028 (10)0.0138 (11)
Cl30.0593 (15)0.0369 (12)0.0756 (19)0.0015 (10)0.0199 (13)0.0112 (12)
Cl40.0455 (13)0.0652 (15)0.0456 (14)0.0080 (11)0.0014 (10)0.0210 (12)
O10.051 (4)0.031 (3)0.043 (4)0.006 (3)0.011 (3)0.013 (3)
O20.067 (4)0.024 (3)0.038 (4)0.004 (3)0.004 (3)0.010 (3)
O30.030 (3)0.028 (3)0.064 (4)0.001 (2)0.003 (3)0.013 (3)
O40.034 (3)0.032 (3)0.051 (4)0.004 (2)0.010 (3)0.014 (3)
O50.062 (4)0.059 (4)0.035 (4)0.022 (3)0.011 (3)0.018 (3)
O60.048 (4)0.053 (4)0.043 (4)0.009 (3)0.012 (3)0.019 (3)
O70.064 (4)0.049 (4)0.044 (4)0.020 (3)0.012 (3)0.019 (3)
O80.053 (4)0.039 (3)0.040 (4)0.004 (3)0.007 (3)0.013 (3)
O90.119 (8)0.136 (8)0.053 (6)0.032 (6)0.030 (5)0.004 (6)
O100.059 (5)0.097 (6)0.071 (6)0.013 (4)0.026 (4)0.003 (5)
O110.050 (5)0.089 (6)0.142 (9)0.001 (4)0.028 (5)0.064 (6)
O120.085 (6)0.055 (5)0.131 (9)0.003 (4)0.029 (6)0.036 (5)
O130.073 (5)0.043 (4)0.083 (6)0.009 (3)0.013 (4)0.017 (4)
O140.069 (5)0.051 (4)0.116 (7)0.014 (4)0.012 (5)0.031 (5)
O150.045 (4)0.116 (7)0.076 (6)0.014 (4)0.016 (4)0.016 (5)
O160.089 (6)0.080 (5)0.054 (5)0.003 (4)0.018 (4)0.019 (4)
N10.035 (4)0.037 (4)0.080 (6)0.004 (3)0.002 (4)0.024 (4)
N20.042 (4)0.034 (4)0.049 (5)0.004 (3)0.008 (3)0.017 (3)
N30.047 (4)0.042 (4)0.045 (5)0.013 (3)0.007 (3)0.012 (4)
N40.048 (4)0.036 (4)0.044 (5)0.003 (3)0.002 (3)0.004 (3)
N50.037 (4)0.064 (5)0.043 (5)0.002 (4)0.011 (3)0.016 (4)
N60.046 (4)0.050 (4)0.029 (4)0.001 (3)0.001 (3)0.009 (3)
N70.051 (5)0.046 (4)0.045 (5)0.005 (3)0.005 (4)0.008 (4)
N80.047 (5)0.048 (5)0.062 (6)0.015 (3)0.021 (4)0.020 (4)
C10.043 (5)0.035 (5)0.040 (5)0.012 (4)0.003 (4)0.010 (4)
C20.062 (6)0.054 (6)0.043 (6)0.005 (5)0.011 (5)0.021 (5)
C30.083 (9)0.100 (9)0.056 (8)0.036 (7)0.025 (6)0.013 (7)
C40.090 (10)0.127 (11)0.038 (7)0.001 (8)0.000 (6)0.014 (7)
C50.033 (5)0.039 (5)0.042 (5)0.001 (3)0.002 (4)0.011 (4)
C60.032 (5)0.033 (4)0.058 (6)0.006 (3)0.002 (4)0.006 (4)
C70.047 (6)0.080 (8)0.079 (9)0.019 (5)0.015 (6)0.013 (7)
C80.083 (9)0.143 (12)0.057 (8)0.069 (9)0.016 (7)0.021 (8)
C90.053 (6)0.043 (5)0.030 (5)0.005 (4)0.001 (4)0.006 (4)
C100.042 (5)0.060 (6)0.045 (6)0.014 (4)0.010 (4)0.010 (5)
C120.087 (10)0.155 (14)0.080 (11)0.012 (10)0.041 (8)0.022 (10)
C130.050 (6)0.049 (6)0.037 (5)0.012 (4)0.005 (4)0.004 (4)
C140.111 (10)0.064 (7)0.056 (8)0.038 (7)0.024 (7)0.019 (6)
C150.173 (16)0.112 (12)0.095 (12)0.079 (12)0.008 (11)0.027 (10)
Geometric parameters (Å, º) top
Pt1—Pt22.9881 (4)N4—H4A0.8900
Pt1—Pt1i3.2619 (6)N4—H4B0.8900
Pt3—Pt43.0246 (4)N4—H4C0.8900
Pt4—Pt4ii3.3049 (6)N5—H5A0.8900
Pt2—Pt34.5478 (5)N5—H5B0.8900
Pt1—N12.037 (7)N5—H5C0.8900
Pt1—N22.023 (7)N6—H6A0.8900
Pt1—O12.034 (6)N6—H6B0.8900
Pt1—O32.044 (5)N6—H6C0.8900
Pt2—N32.016 (6)N7—H7A0.8900
Pt2—N42.002 (7)N7—H7B0.8900
Pt2—O22.031 (6)N7—H7C0.8900
Pt2—O42.023 (5)N8—H8A0.8900
Pt3—N52.017 (7)N8—H8B0.8900
Pt3—N62.011 (7)N8—H8C0.8900
Pt3—O52.035 (6)C1—C21.517 (12)
Pt3—O72.027 (6)C2—C31.488 (13)
Pt4—N72.020 (7)C2—C41.502 (14)
Pt4—N82.033 (7)C2—H20.9800
Pt4—O62.055 (6)C3—H3D0.9600
Pt4—O82.032 (6)C3—H3E0.9600
Cl1—O91.410 (8)C3—H3F0.9600
Cl1—O121.416 (7)C4—H4D0.9600
Cl1—O101.421 (7)C4—H4E0.9600
Cl1—O111.432 (7)C4—H4F0.9600
Cl2—O151.411 (7)C5—C61.518 (11)
Cl2—O141.420 (7)C6—C81.470 (14)
Cl2—O161.424 (7)C6—C71.489 (13)
Cl2—O131.432 (6)C6—H60.9800
Cl3—O17B1.404 (9)C7—H7D0.9600
Cl3—O20A1.408 (8)C7—H7E0.9600
Cl3—O19A1.421 (8)C7—H7F0.9600
Cl3—O19B1.421 (9)C8—H8D0.9600
Cl3—O20B1.422 (9)C8—H8E0.9600
Cl3—O18A1.428 (8)C8—H8F0.9600
Cl3—O17A1.437 (8)C9—C101.513 (12)
Cl3—O18B1.446 (9)C10—C121.474 (16)
Cl4—O23A1.408 (8)C10—C11A1.56 (3)
Cl4—O22A1.408 (8)C10—C11B1.54 (3)
Cl4—O22B1.418 (9)C11A—H11A0.9600
Cl4—O23B1.424 (9)C11A—H11B0.9600
Cl4—O24B1.427 (9)C11A—H11C0.9600
Cl4—O21B1.432 (9)C11B—H11D0.9600
Cl4—O24A1.444 (8)C11B—H11E0.9600
Cl4—O21A1.472 (8)C11B—H11F0.9600
O1—C11.265 (9)C12—H12A0.9600
O2—C11.241 (10)C12—H12B0.9600
O3—C51.290 (9)C12—H12C0.9600
O4—C51.241 (9)C13—C141.494 (13)
O5—C91.251 (10)C14—C151.459 (16)
O6—C91.242 (10)C14—C16A1.12 (3)
O7—C131.263 (10)C14—C16B1.57 (3)
O8—C131.265 (10)C15—H15A0.9600
N1—H1A0.8900C15—H15B0.9600
N1—H1B0.8900C15—H15C0.9600
N1—H1C0.8900C16A—H16A0.9600
N2—H2A0.8900C16A—H16B0.9600
N2—H2B0.8900C16A—H16C0.9600
N2—H2C0.8900C16B—H16D0.9600
N3—H3A0.8900C16B—H16E0.9600
N3—H3B0.8900C16B—H16F0.9600
N3—H3C0.8900
Pt2—Pt1—Pt1i161.515 (18)H3A—N3—H3C109.5
Pt3—Pt4—Pt4ii155.255 (19)H3B—N3—H3C109.5
N2—Pt1—O1175.1 (2)Pt2—N4—H4A109.5
N2—Pt1—N191.1 (3)Pt2—N4—H4B109.5
O1—Pt1—N190.0 (3)H4A—N4—H4B109.5
N2—Pt1—O389.2 (3)Pt2—N4—H4C109.5
O1—Pt1—O389.3 (2)H4A—N4—H4C109.5
N1—Pt1—O3175.6 (2)H4B—N4—H4C109.5
N2—Pt1—Pt2103.81 (18)Pt3—N5—H5A109.5
O1—Pt1—Pt280.52 (15)Pt3—N5—H5B109.5
N1—Pt1—Pt2104.57 (19)H5A—N5—H5B109.5
O3—Pt1—Pt279.64 (14)Pt3—N5—H5C109.5
N2—Pt1—Pt1i85.16 (18)H5A—N5—H5C109.5
O1—Pt1—Pt1i90.03 (15)H5B—N5—H5C109.5
N1—Pt1—Pt1i91.18 (19)Pt3—N6—H6A109.5
O3—Pt1—Pt1i84.42 (14)Pt3—N6—H6B109.5
N4—Pt2—N389.8 (3)H6A—N6—H6B109.5
N4—Pt2—O489.1 (3)Pt3—N6—H6C109.5
N3—Pt2—O4174.8 (2)H6A—N6—H6C109.5
N4—Pt2—O2173.4 (2)H6B—N6—H6C109.5
N3—Pt2—O290.5 (3)Pt4—N7—H7A109.5
O4—Pt2—O290.0 (2)Pt4—N7—H7B109.5
N4—Pt2—Pt1108.4 (2)H7A—N7—H7B109.5
N3—Pt2—Pt1105.3 (2)Pt4—N7—H7C109.5
O4—Pt2—Pt179.79 (14)H7A—N7—H7C109.5
O2—Pt2—Pt177.82 (14)H7B—N7—H7C109.5
N4—Pt2—Pt3114.6 (2)Pt4—N8—H8A109.5
N3—Pt2—Pt3104.5 (2)Pt4—N8—H8B109.5
O4—Pt2—Pt371.47 (16)H8A—N8—H8B109.5
O2—Pt2—Pt359.04 (16)Pt4—N8—H8C109.5
Pt1—Pt2—Pt3126.901 (12)H8A—N8—H8C109.5
N6—Pt3—N591.4 (3)H8B—N8—H8C109.5
N6—Pt3—O788.9 (3)O2—C1—O1125.3 (8)
N5—Pt3—O7175.7 (3)O2—C1—C2116.3 (8)
N6—Pt3—O5174.3 (3)O1—C1—C2118.3 (8)
N5—Pt3—O587.8 (3)C3—C2—C4111.4 (10)
O7—Pt3—O591.5 (3)C3—C2—C1114.3 (9)
N6—Pt3—Pt4108.14 (19)C4—C2—C1108.5 (8)
N5—Pt3—Pt4105.3 (2)C3—C2—H2107.5
O7—Pt3—Pt478.73 (16)C4—C2—H2107.5
O5—Pt3—Pt477.52 (16)C1—C2—H2107.5
N6—Pt3—Pt253.38 (19)C2—C3—H3D109.5
N5—Pt3—Pt255.0 (2)C2—C3—H3E109.5
O7—Pt3—Pt2122.30 (17)H3D—C3—H3E109.5
O5—Pt3—Pt2122.07 (17)C2—C3—H3F109.5
Pt4—Pt3—Pt2147.371 (13)H3D—C3—H3F109.5
N7—Pt4—O8176.0 (3)H3E—C3—H3F109.5
N7—Pt4—N891.5 (3)C2—C4—H4D109.5
O8—Pt4—N888.1 (3)C2—C4—H4E109.5
N7—Pt4—O688.8 (3)H4D—C4—H4E109.5
O8—Pt4—O691.2 (3)C2—C4—H4F109.5
N8—Pt4—O6174.5 (3)H4D—C4—H4F109.5
N7—Pt4—Pt3105.4 (2)H4E—C4—H4F109.5
O8—Pt4—Pt378.47 (15)O4—C5—O3126.8 (7)
N8—Pt4—Pt3106.4 (2)O4—C5—C6117.1 (7)
O6—Pt4—Pt378.81 (16)O3—C5—C6116.1 (7)
N7—Pt4—Pt4ii85.8 (2)C8—C6—C7112.5 (9)
O8—Pt4—Pt4ii90.33 (16)C8—C6—C5111.0 (8)
N8—Pt4—Pt4ii95.1 (2)C7—C6—C5110.0 (8)
O6—Pt4—Pt4ii79.45 (16)C8—C6—H6107.7
O9—Cl1—O12110.2 (5)C7—C6—H6107.7
O9—Cl1—O10106.8 (5)C5—C6—H6107.7
O12—Cl1—O10112.2 (5)C6—C7—H7D109.5
O9—Cl1—O11111.3 (6)C6—C7—H7E109.5
O12—Cl1—O11108.4 (5)H7D—C7—H7E109.5
O10—Cl1—O11108.0 (5)C6—C7—H7F109.5
O15—Cl2—O14109.5 (5)H7D—C7—H7F109.5
O15—Cl2—O16109.7 (5)H7E—C7—H7F109.5
O14—Cl2—O16111.8 (5)C6—C8—H8D109.5
O15—Cl2—O13109.3 (5)C6—C8—H8E109.5
O14—Cl2—O13108.0 (4)H8D—C8—H8E109.5
O16—Cl2—O13108.5 (5)C6—C8—H8F109.5
O20A—Cl3—O19A111.2 (6)H8D—C8—H8F109.5
O17B—Cl3—O19B110.3 (7)H8E—C8—H8F109.5
O17B—Cl3—O20B110.0 (11)O6—C9—O5125.8 (9)
O19B—Cl3—O20B114.7 (11)O6—C9—C10115.6 (8)
O20A—Cl3—O18A109.6 (6)O5—C9—C10118.6 (8)
O19A—Cl3—O18A109.3 (6)C12—C10—C9106.8 (9)
O20A—Cl3—O17A109.5 (6)C12—C10—C11B98.7 (14)
O19A—Cl3—O17A109.0 (6)C9—C10—C11B109.5 (14)
O18A—Cl3—O17A108.3 (6)C12—C10—C11A121.5 (14)
O17B—Cl3—O18B109.2 (7)C9—C10—C11A112.5 (14)
O19B—Cl3—O18B106.7 (7)C10—C11A—H11A109.5
O20B—Cl3—O18B105.6 (11)C10—C11A—H11B109.5
O23A—Cl4—O22A113.6 (6)C10—C11A—H11C109.5
O22B—Cl4—O23B104.0 (12)C10—C11B—H11D109.5
O22B—Cl4—O24B105.6 (11)C10—C11B—H11E109.5
O23B—Cl4—O24B114.8 (12)H11D—C11B—H11E109.5
O22B—Cl4—O21B109.1 (12)C10—C11B—H11F109.5
O23B—Cl4—O21B111.8 (12)H11D—C11B—H11F109.5
O24B—Cl4—O21B111.0 (12)H11E—C11B—H11F109.5
O23A—Cl4—O24A110.6 (6)C10—C12—H12A109.5
O22A—Cl4—O24A109.4 (6)C10—C12—H12B109.5
O23A—Cl4—O21A107.6 (6)H12A—C12—H12B109.5
O22A—Cl4—O21A108.7 (6)C10—C12—H12C109.5
O24A—Cl4—O21A106.6 (6)H12A—C12—H12C109.5
C1—O1—Pt1125.9 (6)H12B—C12—H12C109.5
C1—O2—Pt2130.0 (5)O7—C13—O8126.6 (8)
C5—O3—Pt1125.8 (5)O7—C13—C14116.6 (9)
C5—O4—Pt2127.8 (5)O8—C13—C14116.8 (8)
C9—O5—Pt3128.6 (6)C16A—C14—C15124 (2)
C9—O6—Pt4126.4 (6)C16A—C14—C13122 (2)
C13—O7—Pt3126.0 (6)C15—C14—C13112.9 (11)
C13—O8—Pt4126.9 (5)C15—C14—C16B112.0 (15)
Pt1—N1—H1A109.5C13—C14—C16B103.6 (15)
Pt1—N1—H1B109.5C14—C15—H15A109.5
H1A—N1—H1B109.5C14—C15—H15B109.5
Pt1—N1—H1C109.5H15A—C15—H15B109.5
H1A—N1—H1C109.5C14—C15—H15C109.5
H1B—N1—H1C109.5H15A—C15—H15C109.5
Pt1—N2—H2A109.5H15B—C15—H15C109.5
Pt1—N2—H2B109.5C14—C16A—H16A109.5
H2A—N2—H2B109.5C14—C16A—H16B109.5
Pt1—N2—H2C109.5C14—C16A—H16C109.5
H2A—N2—H2C109.5C14—C16B—H16D109.5
H2B—N2—H2C109.5C14—C16B—H16E109.5
Pt2—N3—H3A109.5H16D—C16B—H16E109.5
Pt2—N3—H3B109.5C14—C16B—H16F109.5
H3A—N3—H3B109.5H16D—C16B—H16F109.5
Pt2—N3—H3C109.5H16E—C16B—H16F109.5
N2—Pt1—Pt2—N42.2 (3)O1—C1—C2—C495.7 (10)
N1—Pt1—Pt2—N32.1 (3)O4—C5—C6—C859.4 (12)
O3—Pt1—Pt2—O41.2 (3)O3—C5—C6—C8119.1 (10)
O1—Pt1—Pt2—O22.5 (2)O4—C5—C6—C765.8 (11)
N5—Pt3—Pt4—N712.4 (3)O3—C5—C6—C7115.8 (9)
O7—Pt3—Pt4—O811.4 (3)O6—C9—C10—C1294.8 (11)
N6—Pt3—Pt4—N812.0 (3)O5—C9—C10—C1286.4 (12)
O5—Pt3—Pt4—O610.9 (3)O6—C9—C10—C11B159.2 (14)
O2—C1—C2—C3153.2 (9)O5—C9—C10—C11B19.6 (17)
O1—C1—C2—C329.3 (12)O6—C9—C10—C11A129.5 (14)
O2—C1—C2—C481.8 (11)O5—C9—C10—C11A49.4 (16)
Symmetry codes: (i) x, y+1, z+1; (ii) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1B···O21A0.892.363.222 (17)162
N1—H1B···O24B0.892.603.117 (19)118
N2—H2A···O18B0.892.223.065 (17)159
N2—H2A···O20A0.892.373.135 (18)144
N2—H2B···O21A0.892.293.135 (18)158
N3—H3C···O130.892.473.128 (9)131
N3—H3B···O24A0.892.132.970 (16)157
N3—H3B···O24B0.891.922.768 (16)159
N4—H4A···O18A0.892.112.716 (11)125
N4—H4C···O23A0.892.072.963 (16)176
N5—H5A···O20.892.713.110 (8)108
N5—H5B···O130.892.313.057 (11)141
N6—H6C···O40.892.383.248 (8)165
N6—H6A···O110.892.362.943 (10)123
N6—H6A···O120.892.503.348 (11)160
N6—H6B···O160.892.413.231 (10)154
N8—H8B···O110.892.162.963 (11)149
N1—H1C···O14iii0.892.213.005 (9)149
N1—H1A···O3i0.892.343.105 (8)144
N2—H2C···O1i0.892.283.093 (8)152
N3—H3C···O10iv0.892.293.041 (11)142
N3—H3A···O10v0.892.162.998 (11)157
N4—H4B···O11iv0.892.593.151 (11)122
N4—H4A···O15iv0.892.483.013 (10)119
N5—H5C···O22Biii0.892.303.133 (19)156
N5—H5C···O24Aiii0.892.403.172 (16)145
N5—H5A···O9v0.892.443.213 (13)146
N7—H7B···O22Aiii0.892.343.185 (17)160
N7—H7B···O22Biii0.892.162.91 (2)142
N7—H7A···O8ii0.892.473.167 (9)135
N7—H7A···O19Aiv0.892.392.938 (15)120
N8—H8C···O6ii0.892.393.109 (9)138
N8—H8A···O19Aiv0.892.443.155 (14)138
N8—H8A···O19Biv0.891.922.759 (12)156
Symmetry codes: (i) x, y+1, z+1; (ii) x+1, y, z; (iii) x, y, z+1; (iv) x+1, y, z+1; (v) x1, y, z.
 

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