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The title compound, {[Pt2Cl2(C2H8N2)4](BF4)4}n or [PtII(C2H8N2)2][PtIVCl2(C2H8N2)2](BF4)4, has a linear chain structure composed of square-planar [Pt(en)2]2+ and elongated octa­hedral trans-[PtCl2(en)2]2+ cations (en is ethyl­ene­diamine) stacked alternately, bridged by the Cl atoms, along the c axis. The Cl atom bridging the adjacent Pt atoms is disordered over two sites along the ...Cl—PtIV—Cl...PtII... chain, which lies on a twofold axis. The PtIV—Cl and PtII...Cl bond distances are 2.319 (3) and 3.052 (3) Å, respectively. A structural parameter indicating the mixed-valence state of the Pt atom, expressed by δ = (PtIV—Cl)/(PtII...Cl), is 0.760.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805004113/hb6153sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805004113/hb6153Isup2.hkl
Contains datablock I

CCDC reference: 269577

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.011 Å
  • Disorder in main residue
  • R factor = 0.026
  • wR factor = 0.068
  • Data-to-parameter ratio = 19.6

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for B
Author Response: The U(eq) of the B atom of the counter-anion, BF~4~^-^ is relatively small comparing with the U(eq) of the atom F3. The U(eq) of the atom F3 is too large due to the disorder of the BF~4~^-^ ion.

Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . CL PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.66 PLAT213_ALERT_2_C Atom F3 has ADP max/min Ratio ............. 3.20 oblate PLAT301_ALERT_3_C Main Residue Disorder ......................... 14.00 Perc. PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11
Alert level G ABSTM02_ALERT_3_G The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.077 0.255 Tmin and Tmax expected: 0.046 0.209 RR = 1.366 Please check that your absorption correction is appropriate.
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: Rigaku/AFC Diffractometer Control Software (Rigaku, 1987); cell refinement: Rigaku/AFC Diffractometer Control Software; data reduction: local program; program(s) used to solve structure: UNICS3 (Sakurai & Kobayashi, 1979); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: Please provide missing details.

catena-poly[[[bis(ethylenediamine)platinum(II)]-µ-chloro- [bis(ethylenediamine)platinum(IV)]-µ-chloro] tetrakis(tetrafluoroborate)] top
Crystal data top
[Pt2Cl2(C2H8N2)4](BF4)4Dx = 2.523 Mg m3
Mr = 1048.74Melting point: not measured K
Orthorhombic, IbamMo Kα radiation, λ = 0.71069 Å
Hall symbol: -I 2 2cCell parameters from 25 reflections
a = 9.580 (2) Åθ = 10.5–14.8°
b = 13.416 (2) ŵ = 10.44 mm1
c = 10.743 (2) ÅT = 295 K
V = 1380.7 (4) Å3Plate, intense red
Z = 20.33 × 0.30 × 0.15 mm
F(000) = 980
Data collection top
Rigaku AFC-5S
diffractometer
821 reflections with F2 > 2σ(F2)
Radiation source: X-ray tubeRint = 0.023
Graphite monochromatorθmax = 32.5°, θmin = 2.6°
θ/2θ scansh = 1414
Absorption correction: gaussian
(Coppens et al., 1965)
k = 020
Tmin = 0.077, Tmax = 0.255l = 016
3523 measured reflections3 standard reflections every 50 reflections
1311 independent reflections intensity decay: none
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)] = 0.026H-atom parameters constrained
wR(F2) = 0.068 w = 1/[σ2(Fo2) + (0.0407P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max < 0.001
1311 reflectionsΔρmax = 3.52 e Å3
67 parametersΔρmin = 1.33 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: heavy-atom methodExtinction coefficient: 0.0063 (3)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Pt0.00000.00000.25000.02551 (11)
Cl0.00000.00000.0341 (2)0.0348 (5)0.50
N0.1600 (4)0.1013 (3)0.2481 (4)0.0399 (7)
H10.16860.12800.17160.060*
H20.14220.15080.30240.060*
C0.2911 (6)0.0495 (6)0.2832 (6)0.0546 (15)
H30.29490.03950.37260.082*
H40.37150.08870.25830.082*
B0.4161 (13)0.2019 (9)0.00000.056 (2)
F10.4757 (6)0.2377 (5)0.1052 (5)0.0960 (18)
F20.456 (2)0.1003 (8)0.00000.092 (4)0.60
F2'0.337 (3)0.1231 (14)0.00000.083 (6)0.40
F30.2852 (17)0.208 (3)0.00000.195 (13)0.60
F3'0.311 (3)0.283 (2)0.00000.153 (13)0.40
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt0.02912 (14)0.02802 (14)0.01940 (14)0.0000.0000.000
Cl0.0427 (11)0.0412 (11)0.0205 (8)0.0043 (19)0.0000.000
N0.0427 (16)0.0402 (16)0.0366 (17)0.0108 (14)0.002 (2)0.005 (2)
C0.036 (2)0.080 (4)0.047 (3)0.016 (3)0.006 (2)0.006 (3)
B0.067 (7)0.057 (6)0.044 (5)0.006 (5)0.0000.000
F10.157 (5)0.078 (3)0.053 (2)0.002 (3)0.020 (2)0.013 (2)
F20.169 (12)0.035 (4)0.073 (8)0.010 (7)0.0000.000
F2'0.14 (2)0.047 (9)0.057 (9)0.040 (11)0.0000.000
F30.031 (5)0.32 (4)0.23 (2)0.007 (16)0.0000.000
F3'0.09 (2)0.11 (2)0.26 (3)0.029 (16)0.0000.000
Geometric parameters (Å, º) top
Pt—N2.049 (4)C—H30.9700
Pt—Cl2.319 (3)C—H40.9700
Cl—Pti3.052 (3)B—F31.256 (19)
N—C1.485 (8)B—F2'1.301 (19)
N—H10.9000B—F11.355 (8)
N—H20.9000B—F21.415 (16)
C—Cii1.506 (15)B—F3'1.48 (4)
Niii—Pt—N178.9 (2)N—C—H3110.3
N—Pt—Nii83.1 (2)Cii—C—H3110.3
N—Pt—Niv96.9 (2)N—C—H4110.3
N—Pt—Cliv90.57 (12)Cii—C—H4110.3
N—Pt—Cl89.43 (12)H3—C—H4108.6
Cliv—Pt—Cl180.0F3—B—F1113.6 (10)
Pt—Cl—Pti180.0F2'—B—F1122.3 (6)
C—N—Pt108.6 (3)F3—B—F1v113.6 (10)
C—N—H1110.0F1—B—F1v113.1 (10)
Pt—N—H1110.0F3—B—F2109.2 (17)
C—N—H2110.0F1—B—F2103.1 (9)
Pt—N—H2110.0F2'—B—F3'101.4 (18)
H1—N—H2108.3F1—B—F3'91.6 (8)
N—C—Cii107.0 (4)
Symmetry codes: (i) x, y, z; (ii) x, y, z+1/2; (iii) x, y, z; (iv) x, y, z+1/2; (v) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N—H2···F1vi0.902.122.973 (8)158
N—H1···F30.902.413.252 (16)157
N—H2···F3vi0.902.353.134 (15)146
N—H1···F20.902.453.172 (17)137
Symmetry code: (vi) x+1/2, y+1/2, z+1/2.
 

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