cis-Dichloro­bis(4-methyl­pyridine-κN)platinum(II)

In the title mol­ecule, cis-[PtCl₂(C₆H₇N)₂], the Pt^II coordination plane has a distorted structure in which the cis-PtCl₂ unit is tilted by 4.3 (2)° with respect to the cis-PtN₂ unit. The two pyridyl planes are inclined at angles of 64.8 (1) and 77.5 (2)° with respect to the cis-PtN₂ unit, which is partly inter­preted in terms of the inter­molecular C—H(meth­yl)...π(pyridine) inter­actions in the crystal structure.

Key indicators

• Single-crystal X-ray study
• T = 113 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.031
• wR factor = 0.087
• Data-to-parameter ratio = 20.0

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.97

Alert level G
ABSTM02_ALERT_3_G  The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
            Tmin and Tmax reported:      0.090     0.271
            Tmin and Tmax expected:      0.072     0.271
            RR =      1.261
            Please check that your absorption correction is appropriate.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   1 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: CrystalClear (Rigaku/MSC, 2002); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku/MSC, 2003); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: KENX (Sakai, 2004); software used to prepare material for publication: SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX and ORTEPII (Johnson, 1976).

cis-dichlorobis(4-metylpyridine-κN)platinum(II)

Crystal data

[PtCl2(C6H7N)2]	F(000) = 1696
Mr = 452.24	Dx = 2.141 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -C 2yc	Cell parameters from 3970 reflections
a = 14.105 (4) Å	θ = 5.8–27.5°
b = 12.530 (3) Å	µ = 10.36 mm^−1
c = 16.644 (4) Å	T = 113 K
β = 107.429 (2)°	Prism, colorless
V = 2806.5 (12) Å^3	0.38 × 0.23 × 0.13 mm
Z = 8

Data collection

Rigaku Mercury CCD-detector diffractometer	3135 independent reflections
Radiation source: rotating anode	2822 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.063
Detector resolution: 14.7059 pixels mm^-1	θmax = 27.5°, θmin = 6.1°
ω scans	h = −13→18
Absorption correction: numerical (NUMABS; Higashi, 1999)	k = −10→16
Tmin = 0.090, Tmax = 0.271	l = −21→21
10554 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.031	H-atom parameters constrained
wR(F^2) = 0.087	w = 1/[σ^2(Fo^2) + (0.0319P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.16	(Δ/σ)max < 0.001
3135 reflections	Δρmax = 3.49 e Å^−3
157 parameters	Δρmin = −1.82 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00037 (7)

Special details

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. ¹H NMR (301.70 MHz, CDCl₃): δ 2.37 (s, 6H, methyl), 7.11 (d, 4H, pyridyl, J = 6.62 Hz), and 8.61 (d, 4H, pyridyl, J = 6.62 Hz).

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)

5.2875 (0.0120) x + 11.4408 (0.0056) y - 4.4176 (0.0149) z = 2.1080 (0.0017)

* 0.0067 (0.0012) Pt1 * 0.0505 (0.0014) Cl1 * -0.0527 (0.0014) Cl2 * -0.0633 (0.0017) N1 * 0.0588 (0.0017) N2

Rms deviation of fitted atoms = 0.051 (39)

4.9433 (0.0072) x + 11.5177 (0.0040) y - 4.5974 (0.0090) z = 2.0756 (0.0009)

Angle to previous plane (with approximate e.s.d.) = 1.81 (0.08)

* 0.0000 (0.0000) Pt1 * 0.0000 (0.0000) Cl1 * 0.0000 (0.0000) Cl2 - 0.1214 (0.0039) N1 0.0876 (0.0041) N2

Rms deviation of fitted atoms = 0.0000

5.7709 (0.0255) x + 11.3074 (0.0110) y - 4.1833 (0.0299) z = 2.1657 (0.0022)

Angle to previous plane (with approximate e.s.d.) = 4.33 (0.15)

* 0.0000 (0.0000) Pt1 * 0.0000 (0.0000) N1 * 0.0000 (0.0000) N2 0.1079 (0.0047) Cl1 - 0.1401 (0.0044) Cl2

Rms deviation of fitted atoms = 0.0000

- 8.2410 (0.0235) x + 9.6972 (0.0165) y + 6.7922 (0.0291) z = 0.4488 (0.0093)

Angle to previous plane (with approximate e.s.d.) = 64.76 (0.12)

* -0.0114 (0.0032) N1 * -0.0009 (0.0036) C1 * 0.0113 (0.0037) C2 * -0.0097 (0.0035) C3 * -0.0019 (0.0036) C4 * 0.0127 (0.0034) C5 - 0.0042 (0.0084) C6

Rms deviation of fitted atoms = 0.009 (8)

- 1.6381 (0.0298) x + 5.8806 (0.0249) y - 13.3212 (0.0208) z = 0.3676 (0.0077)

Angle to previous plane (with approximate e.s.d.) = 77.46 (0.16)

* -0.0046 (0.0034) N2 * 0.0041 (0.0037) C7 * 0.0022 (0.0040) C8 * -0.0080 (0.0037) C9 * 0.0076 (0.0036) C10 * -0.0014 (0.0036) C11 - 0.0284 (0.0097) C12

Rms deviation of fitted atoms = 0.0053 (52)

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 (Ų)

	x	y	z	Uiso*/Ueq
Pt1	0.132241 (13)	0.131425 (13)	0.019963 (12)	0.01431 (11)
Cl1	0.26328 (9)	0.06027 (10)	−0.01740 (9)	0.0224 (3)
Cl2	0.02860 (11)	0.12157 (10)	−0.11615 (10)	0.0219 (3)
N1	0.2186 (4)	0.1321 (3)	0.1410 (3)	0.0152 (10)
N2	0.0248 (3)	0.2004 (3)	0.0581 (3)	0.0170 (9)
C1	0.3035 (4)	0.1882 (4)	0.1656 (4)	0.0225 (11)
H1	0.3215	0.2314	0.1255	0.027*
C2	0.3647 (4)	0.1850 (4)	0.2462 (4)	0.0226 (11)
H2	0.4236	0.2268	0.2613	0.027*
C3	0.3424 (4)	0.1208 (4)	0.3075 (4)	0.0176 (11)
C4	0.2526 (4)	0.0644 (4)	0.2804 (3)	0.0181 (10)
H4	0.2327	0.0201	0.3188	0.022*
C5	0.1929 (4)	0.0729 (4)	0.1979 (3)	0.0180 (10)
H5	0.1316	0.0354	0.1812	0.022*
C6	0.4102 (4)	0.1161 (4)	0.3974 (4)	0.0221 (12)
H6A	0.4796	0.1202	0.3975	0.033*
H6B	0.3993	0.0488	0.4234	0.033*
H6C	0.3954	0.1761	0.4295	0.033*
C7	0.0417 (4)	0.2967 (4)	0.0979 (3)	0.0203 (11)
H7	0.1037	0.3312	0.1050	0.024*
C8	−0.0275 (4)	0.3451 (4)	0.1280 (4)	0.0244 (12)
H8	−0.0129	0.4123	0.1554	0.029*
C9	−0.1193 (4)	0.2975 (4)	0.1190 (3)	0.0213 (11)
C10	−0.1366 (4)	0.2007 (4)	0.0772 (4)	0.0217 (11)
H10	−0.1989	0.1662	0.0684	0.026*
C11	−0.0647 (4)	0.1532 (4)	0.0481 (3)	0.0177 (10)
H11	−0.0782	0.0861	0.0204	0.021*
C12	−0.1943 (5)	0.3501 (5)	0.1530 (5)	0.0306 (14)
H12A	−0.1696	0.4203	0.1759	0.046*
H12B	−0.2056	0.3058	0.1978	0.046*
H12C	−0.2568	0.3588	0.1077	0.046*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pt1	0.01563 (15)	0.01382 (15)	0.01363 (15)	−0.00108 (6)	0.00462 (10)	−0.00029 (6)
Cl1	0.0232 (6)	0.0234 (6)	0.0239 (7)	0.0015 (5)	0.0119 (5)	−0.0031 (5)
Cl2	0.0243 (7)	0.0227 (7)	0.0160 (7)	−0.0029 (5)	0.0017 (6)	0.0014 (5)
N1	0.019 (2)	0.017 (2)	0.011 (2)	−0.0015 (14)	0.0071 (19)	−0.0034 (15)
N2	0.013 (2)	0.018 (2)	0.020 (2)	0.0008 (15)	0.0038 (17)	0.0015 (18)
C1	0.020 (3)	0.019 (2)	0.031 (3)	−0.006 (2)	0.011 (2)	−0.003 (2)
C2	0.017 (2)	0.023 (3)	0.028 (3)	−0.006 (2)	0.008 (2)	−0.003 (2)
C3	0.019 (3)	0.020 (3)	0.014 (3)	0.0013 (18)	0.006 (2)	−0.002 (2)
C4	0.021 (3)	0.018 (2)	0.016 (3)	−0.0027 (19)	0.007 (2)	−0.001 (2)
C5	0.017 (2)	0.016 (2)	0.022 (3)	−0.0036 (19)	0.007 (2)	−0.002 (2)
C6	0.024 (3)	0.021 (2)	0.018 (3)	−0.003 (2)	0.001 (2)	−0.002 (2)
C7	0.019 (2)	0.019 (2)	0.022 (3)	−0.0019 (19)	0.005 (2)	−0.003 (2)
C8	0.029 (3)	0.019 (2)	0.026 (3)	−0.001 (2)	0.009 (2)	−0.002 (3)
C9	0.024 (3)	0.020 (2)	0.020 (3)	0.009 (2)	0.008 (2)	0.008 (2)
C10	0.019 (3)	0.022 (3)	0.025 (3)	0.000 (2)	0.007 (2)	0.009 (2)
C11	0.019 (3)	0.015 (2)	0.018 (3)	−0.0027 (19)	0.004 (2)	0.001 (2)
C12	0.031 (3)	0.027 (3)	0.040 (4)	0.005 (2)	0.020 (3)	−0.002 (3)

Geometric parameters (Å, º)

Pt1—N2	2.005 (4)	C9—C12	1.494 (7)
Pt1—N1	2.017 (5)	C10—C11	1.383 (7)
Pt1—Cl1	2.2993 (13)	C1—H1	0.9500
Pt1—Cl2	2.3023 (16)	C2—H2	0.9500
N1—C5	1.336 (7)	C4—H4	0.9500
N1—C1	1.343 (6)	C5—H5	0.9500
N2—C11	1.359 (6)	C6—H6A	0.9800
N2—C7	1.363 (6)	C6—H6B	0.9800
C1—C2	1.361 (8)	C6—H6C	0.9800
C2—C3	1.408 (8)	C7—H7	0.9500
C3—C4	1.401 (7)	C8—H8	0.9500
C3—C6	1.517 (8)	C10—H10	0.9500
C4—C5	1.382 (7)	C11—H11	0.9500
C7—C8	1.366 (8)	C12—H12A	0.9800
C8—C9	1.392 (8)	C12—H12B	0.9800
C9—C10	1.384 (7)	C12—H12C	0.9800
Pt1···Cl1^i	4.1394 (15)	C5···C12^iii	3.405 (7)
Pt1···Pt1^i	4.6508 (9)	C7···C6^iv	3.474 (8)
Pt1···H11^ii	2.8554
N2—Pt1—N1	88.24 (18)	C2—C1—H1	119.0
N2—Pt1—Cl1	175.95 (12)	C1—C2—H2	119.4
N1—Pt1—Cl1	88.73 (14)	C3—C2—H2	119.4
N2—Pt1—Cl2	91.01 (13)	C5—C4—H4	119.9
N1—Pt1—Cl2	176.43 (12)	C3—C4—H4	119.9
Cl1—Pt1—Cl2	92.18 (5)	N1—C5—H5	118.9
C5—N1—C1	118.7 (5)	C4—C5—H5	118.9
C5—N1—Pt1	119.7 (4)	C3—C6—H6A	109.5
C1—N1—Pt1	121.6 (4)	C3—C6—H6B	109.5
C11—N2—C7	117.8 (4)	H6A—C6—H6B	109.5
C11—N2—Pt1	122.4 (3)	C3—C6—H6C	109.5
C7—N2—Pt1	119.8 (3)	H6A—C6—H6C	109.5
N1—C1—C2	122.0 (5)	H6B—C6—H6C	109.5
C1—C2—C3	121.2 (5)	N2—C7—H7	119.0
C4—C3—C2	115.6 (5)	C8—C7—H7	119.0
C4—C3—C6	122.7 (5)	C7—C8—H8	119.5
C2—C3—C6	121.7 (5)	C9—C8—H8	119.5
C5—C4—C3	120.2 (5)	C11—C10—H10	119.5
N1—C5—C4	122.2 (5)	C9—C10—H10	119.5
N2—C7—C8	122.1 (5)	N2—C11—H11	119.3
C7—C8—C9	120.9 (5)	C10—C11—H11	119.3
C10—C9—C8	116.6 (5)	C9—C12—H12A	109.5
C10—C9—C12	122.6 (5)	C9—C12—H12B	109.5
C8—C9—C12	120.8 (5)	H12A—C12—H12B	109.5
C11—C10—C9	121.1 (5)	C9—C12—H12C	109.5
N2—C11—C10	121.5 (5)	H12A—C12—H12C	109.5
N1—C1—H1	119.0	H12B—C12—H12C	109.5
C5—N1—C1—C2	1.1 (8)	C11—N2—C7—C8	0.7 (8)
N1—C1—C2—C3	1.1 (8)	N2—C7—C8—C9	0.0 (9)
C1—C2—C3—C4	−1.9 (8)	C7—C8—C9—C10	−1.1 (8)
C1—C2—C3—C6	179.7 (5)	C7—C8—C9—C12	179.2 (6)
C2—C3—C4—C5	0.6 (7)	C8—C9—C10—C11	1.6 (8)
C6—C3—C4—C5	179.0 (5)	C12—C9—C10—C11	−178.7 (5)
C1—N1—C5—C4	−2.4 (7)	C7—N2—C11—C10	−0.1 (7)
C3—C4—C5—N1	1.6 (8)	C9—C10—C11—N2	−1.1 (8)

Symmetry codes: (i) −x+1/2, −y+1/2, −z; (ii) −x, −y, −z; (iii) x+1/2, y−1/2, z; (iv) x−1/2, −y+1/2, z−1/2.