Chloro(dimethyl sulfoxide-κS)[(1R,3S)-1,2,2-trimethyl­cyclo­pentane-1,3-diamine-κ²N,N′]platinum(II) trichloro­(dimethyl sulfoxide-κS)platinum(II)

The mol­ecule of the title compound, [PtCl(C₈H₁₈N₂)(C₂H₆OS)][PtCl₃(C₂H₆OS)], contains one cation and one anion, each with a square-planar coordination around the Pt^II centre. The bond lengths and angles of Pt with N, Cl and S atoms are also typical of diamine dichloro­platinum(II) complexes.

Key indicators

• Single-crystal X-ray study
• T = 296 K
• Mean [sigma](C-C) = 0.009 Å
• R factor = 0.028
• wR factor = 0.063
• Data-to-parameter ratio = 23.3

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          9
PLAT420_ALERT_2_C D-H Without Acceptor       N2     -   H2NA   ...          ?
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          4

Alert level G
CHEMS02_ALERT_1_G  Please check that you have entered the correct
            _publ_requested_category classification of your compound;
            FI or CI or EI for inorganic; FM or CM or EM for metal-organic;
            FO or CO or EO for organic.
            From the CIF: _publ_requested_category   FI
            From the CIF: _chemical_formula_sum:C12 H30 Cl4 N2 O2 Pt2 S2
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           27.49
           From the CIF: _reflns_number_total               5213
           Count of symmetry unique reflns         2960
           Completeness (_total/calc)            176.11%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      2253
           Fraction of Friedel pairs measured     0.761
           Are heavy atom types Z>Si present        yes
PLAT791_ALERT_1_G Confirm the Absolute Configuration of C2     = .          R
PLAT791_ALERT_1_G Confirm the Absolute Configuration of C6     = .          S

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

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

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Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001) and/or ORTEPII (Johnson, 1976)????; software used to prepare material for publication: SHELXL97.

Chloro-(1R,3S)-1,3-diamino-1,2,2-trimethylcyclopentane(dimethyl sulphoxide) platinum(II) trichloro(dimethyl sulphoxide)platinum(II)

Crystal data

[PtCl(C8H18N2)(C2H6OS)][PtCl3(C2H6OS)]	F(000) = 1552
Mr = 830.48	Dx = 2.412 Mg m^−3
Orthorhombic, P212121	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2ab	Cell parameters from 14847 reflections
a = 11.5381 (12) Å	θ = 2.1–27.5°
b = 11.9979 (13) Å	µ = 12.88 mm^−1
c = 16.5192 (18) Å	T = 296 K
V = 2286.8 (4) Å^3	Block, yellow
Z = 4	0.20 × 0.20 × 0.15 mm

Data collection

Bruker SMART 1000 CCD diffractometer	5213 independent reflections
Radiation source: fine-focus sealed tube	4947 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.054
ω scans	θmax = 27.5°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −14→14
Tmin = 0.097, Tmax = 0.149	k = −15→14
14847 measured reflections	l = −10→21

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)] = 0.028	H-atom parameters constrained
wR(F^2) = 0.063	w = 1/[σ^2(Fo^2) + (0.0344P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.02	(Δ/σ)max = 0.001
5213 reflections	Δρmax = 1.90 e Å^−3
224 parameters	Δρmin = −1.39 e Å^−3
0 restraints	Absolute structure: Flack (1983), 2253 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.002 (7)

Special details

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.

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	0.44727 (2)	0.597083 (17)	0.263955 (15)	0.02124 (6)
Pt2	0.89949 (2)	0.47131 (2)	0.336440 (17)	0.02671 (7)
Cl1	0.33257 (16)	0.47504 (14)	0.19195 (11)	0.0373 (4)
Cl2	1.05457 (16)	0.53059 (15)	0.41239 (12)	0.0406 (4)
Cl3	0.82995 (14)	0.65267 (15)	0.34050 (16)	0.0450 (5)
Cl4	0.74391 (16)	0.42142 (18)	0.25719 (14)	0.0493 (5)
S1	0.51069 (14)	0.67921 (12)	0.15227 (10)	0.0262 (3)
S2	0.96280 (15)	0.29900 (13)	0.34731 (11)	0.0311 (4)
O1	0.5812 (4)	0.7800 (3)	0.1651 (3)	0.0321 (11)
O2	0.9371 (6)	0.2484 (4)	0.4261 (3)	0.0528 (16)
N1	0.5548 (5)	0.6971 (4)	0.3308 (3)	0.0233 (10)
H1NA	0.6281	0.6675	0.3276	0.028*
H1NB	0.5572	0.7656	0.3058	0.028*
N2	0.3802 (4)	0.5218 (4)	0.3668 (3)	0.0238 (11)
H2NA	0.3030	0.5082	0.3567	0.029*
H2NB	0.4156	0.4533	0.3713	0.029*
C1	0.3341 (6)	0.4932 (5)	0.5091 (5)	0.0333 (16)
H1A	0.2520	0.4820	0.4963	0.050*
H1B	0.3414	0.5229	0.5641	0.050*
H1C	0.3751	0.4219	0.5054	0.050*
C2	0.3870 (5)	0.5759 (5)	0.4488 (4)	0.0229 (13)
C3	0.5152 (5)	0.6088 (5)	0.4670 (4)	0.0218 (12)
C4	0.5267 (6)	0.6394 (6)	0.5563 (5)	0.0342 (16)
H4A	0.6054	0.6665	0.5669	0.051*
H4B	0.5114	0.5734	0.5896	0.051*
H4C	0.4706	0.6979	0.5697	0.051*
C5	0.6033 (5)	0.5162 (5)	0.4492 (4)	0.0294 (14)
H5A	0.6065	0.5028	0.3907	0.044*
H5B	0.5797	0.4477	0.4769	0.044*
H5C	0.6800	0.5391	0.4685	0.044*
C6	0.5293 (6)	0.7167 (5)	0.4177 (4)	0.0260 (14)
H6	0.5915	0.7639	0.4422	0.031*
C7	0.4119 (6)	0.7762 (5)	0.4249 (4)	0.0288 (14)
H7A	0.4147	0.8335	0.4680	0.035*
H7B	0.3915	0.8129	0.3732	0.035*
C8	0.3231 (6)	0.6858 (5)	0.4459 (5)	0.0306 (15)
H8A	0.2868	0.7018	0.4989	0.037*
H8B	0.2614	0.6833	0.4042	0.037*
C9	0.5896 (8)	0.5858 (6)	0.0919 (5)	0.0427 (18)
H9A	0.6192	0.6249	0.0441	0.064*
H9B	0.5389	0.5246	0.0748	0.064*
H9C	0.6546	0.5557	0.1232	0.064*
C10	0.3941 (7)	0.7142 (5)	0.0887 (5)	0.0348 (16)
H10A	0.3485	0.7739	0.1137	0.052*
H10B	0.3448	0.6486	0.0806	0.052*
H10C	0.4239	0.7397	0.0363	0.052*
C11	1.1144 (7)	0.2903 (7)	0.3340 (6)	0.047 (2)
H11A	1.1534	0.3252	0.3802	0.071*
H11B	1.1364	0.3289	0.2841	0.071*
H11C	1.1374	0.2118	0.3304	0.071*
C12	0.9112 (7)	0.2069 (7)	0.2713 (6)	0.049 (2)
H12A	0.9421	0.1319	0.2811	0.074*
H12B	0.9368	0.2331	0.2181	0.074*
H12C	0.8264	0.2046	0.2729	0.074*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pt1	0.02868 (11)	0.01930 (10)	0.01575 (12)	−0.00284 (8)	−0.00356 (10)	0.00104 (9)
Pt2	0.02352 (11)	0.03567 (13)	0.02092 (13)	−0.00355 (10)	0.00156 (10)	0.00273 (12)
Cl1	0.0565 (11)	0.0293 (8)	0.0260 (9)	−0.0137 (7)	−0.0169 (8)	0.0031 (8)
Cl2	0.0357 (8)	0.0400 (8)	0.0460 (11)	−0.0070 (8)	−0.0107 (9)	−0.0070 (8)
Cl3	0.0293 (8)	0.0403 (9)	0.0653 (15)	0.0003 (6)	0.0054 (10)	0.0112 (10)
Cl4	0.0370 (9)	0.0743 (12)	0.0367 (11)	0.0002 (8)	−0.0129 (9)	−0.0081 (11)
S1	0.0396 (8)	0.0213 (6)	0.0176 (8)	−0.0020 (5)	−0.0021 (7)	0.0011 (6)
S2	0.0361 (9)	0.0347 (8)	0.0224 (9)	−0.0036 (6)	0.0003 (7)	−0.0036 (7)
O1	0.047 (3)	0.025 (2)	0.025 (3)	−0.0122 (18)	0.001 (2)	−0.001 (2)
O2	0.095 (5)	0.038 (3)	0.025 (3)	−0.002 (3)	0.007 (3)	0.005 (2)
N1	0.031 (2)	0.023 (2)	0.016 (3)	−0.006 (2)	−0.004 (3)	0.004 (2)
N2	0.023 (2)	0.023 (2)	0.025 (3)	−0.0047 (19)	−0.003 (2)	0.003 (2)
C1	0.029 (3)	0.043 (4)	0.028 (4)	−0.009 (3)	0.005 (3)	0.008 (3)
C2	0.023 (3)	0.027 (3)	0.019 (3)	−0.004 (2)	0.000 (3)	0.002 (3)
C3	0.025 (3)	0.021 (3)	0.019 (3)	0.000 (2)	−0.001 (2)	0.002 (3)
C4	0.036 (4)	0.043 (4)	0.024 (4)	−0.004 (3)	−0.010 (3)	0.001 (3)
C5	0.028 (3)	0.036 (3)	0.024 (4)	0.007 (3)	−0.001 (3)	0.007 (3)
C6	0.037 (4)	0.022 (3)	0.018 (3)	−0.006 (2)	−0.010 (3)	0.000 (3)
C7	0.044 (4)	0.024 (3)	0.018 (3)	0.003 (3)	−0.001 (3)	−0.002 (3)
C8	0.029 (3)	0.031 (3)	0.032 (4)	0.008 (2)	0.001 (3)	0.000 (3)
C9	0.059 (5)	0.041 (4)	0.028 (4)	0.010 (4)	0.001 (4)	−0.004 (4)
C10	0.055 (4)	0.025 (3)	0.025 (4)	−0.003 (3)	−0.011 (4)	0.005 (3)
C11	0.046 (4)	0.048 (4)	0.049 (5)	0.006 (3)	−0.001 (4)	−0.005 (4)
C12	0.039 (4)	0.055 (4)	0.054 (6)	−0.013 (3)	0.007 (4)	−0.029 (4)

Geometric parameters (Å, º)

Pt1—N1	2.049 (5)	C3—C5	1.534 (8)
Pt1—N2	2.074 (5)	C3—C6	1.538 (8)
Pt1—S1	2.2159 (16)	C4—H4A	0.9800
Pt1—Cl1	2.3044 (16)	C4—H4B	0.9800
Pt2—S2	2.2000 (17)	C4—H4C	0.9800
Pt2—Cl2	2.2982 (18)	C5—H5A	0.9800
Pt2—Cl4	2.3010 (19)	C5—H5B	0.9800
Pt2—Cl3	2.3201 (18)	C5—H5C	0.9800
S1—O1	1.473 (4)	C6—C7	1.535 (9)
S1—C9	1.755 (8)	C6—H6	1.0000
S1—C10	1.758 (7)	C7—C8	1.532 (9)
S2—O2	1.466 (6)	C7—H7A	0.9900
S2—C11	1.766 (8)	C7—H7B	0.9900
S2—C12	1.775 (8)	C8—H8A	0.9900
N1—C6	1.484 (8)	C8—H8B	0.9900
N1—H1NA	0.9200	C9—H9A	0.9800
N1—H1NB	0.9200	C9—H9B	0.9800
N2—C2	1.505 (8)	C9—H9C	0.9800
N2—H2NA	0.9200	C10—H10A	0.9800
N2—H2NB	0.9200	C10—H10B	0.9800
C1—C2	1.532 (9)	C10—H10C	0.9800
C1—H1A	0.9800	C11—H11A	0.9800
C1—H1B	0.9800	C11—H11B	0.9800
C1—H1C	0.9800	C11—H11C	0.9800
C2—C8	1.511 (8)	C12—H12A	0.9800
C2—C3	1.560 (8)	C12—H12B	0.9800
C3—C4	1.527 (9)	C12—H12C	0.9800
N1—Pt1—N2	92.3 (2)	C3—C4—H4A	109.5
N1—Pt1—S1	89.32 (15)	C3—C4—H4B	109.5
N2—Pt1—S1	177.37 (14)	H4A—C4—H4B	109.5
N1—Pt1—Cl1	176.41 (15)	C3—C4—H4C	109.5
N2—Pt1—Cl1	86.08 (15)	H4A—C4—H4C	109.5
S1—Pt1—Cl1	92.44 (6)	H4B—C4—H4C	109.5
S2—Pt2—Cl2	89.30 (6)	C3—C5—H5A	109.5
S2—Pt2—Cl4	93.50 (7)	C3—C5—H5B	109.5
Cl2—Pt2—Cl4	176.88 (7)	H5A—C5—H5B	109.5
S2—Pt2—Cl3	173.61 (8)	C3—C5—H5C	109.5
Cl2—Pt2—Cl3	87.89 (7)	H5A—C5—H5C	109.5
Cl4—Pt2—Cl3	89.46 (8)	H5B—C5—H5C	109.5
O1—S1—C9	108.7 (4)	N1—C6—C7	108.9 (5)
O1—S1—C10	108.2 (3)	N1—C6—C3	113.6 (5)
C9—S1—C10	102.1 (4)	C7—C6—C3	104.9 (5)
O1—S1—Pt1	115.3 (2)	N1—C6—H6	109.8
C9—S1—Pt1	111.1 (3)	C7—C6—H6	109.8
C10—S1—Pt1	110.6 (3)	C3—C6—H6	109.8
O2—S2—C11	106.6 (4)	C8—C7—C6	106.2 (5)
O2—S2—C12	107.6 (4)	C8—C7—H7A	110.5
C11—S2—C12	101.9 (4)	C6—C7—H7A	110.5
O2—S2—Pt2	113.2 (2)	C8—C7—H7B	110.5
C11—S2—Pt2	112.0 (3)	C6—C7—H7B	110.5
C12—S2—Pt2	114.6 (3)	H7A—C7—H7B	108.7
C6—N1—Pt1	119.6 (4)	C2—C8—C7	107.4 (5)
C6—N1—H1NA	107.4	C2—C8—H8A	110.2
Pt1—N1—H1NA	107.4	C7—C8—H8A	110.2
C6—N1—H1NB	107.4	C2—C8—H8B	110.2
Pt1—N1—H1NB	107.4	C7—C8—H8B	110.2
H1NA—N1—H1NB	107.0	H8A—C8—H8B	108.5
C2—N2—Pt1	122.0 (3)	S1—C9—H9A	109.5
C2—N2—H2NA	106.8	S1—C9—H9B	109.5
Pt1—N2—H2NA	106.8	H9A—C9—H9B	109.5
C2—N2—H2NB	106.8	S1—C9—H9C	109.5
Pt1—N2—H2NB	106.8	H9A—C9—H9C	109.5
H2NA—N2—H2NB	106.7	H9B—C9—H9C	109.5
C2—C1—H1A	109.5	S1—C10—H10A	109.5
C2—C1—H1B	109.5	S1—C10—H10B	109.5
H1A—C1—H1B	109.5	H10A—C10—H10B	109.5
C2—C1—H1C	109.5	S1—C10—H10C	109.5
H1A—C1—H1C	109.5	H10A—C10—H10C	109.5
H1B—C1—H1C	109.5	H10B—C10—H10C	109.5
N2—C2—C8	108.8 (5)	S2—C11—H11A	109.5
N2—C2—C1	106.5 (5)	S2—C11—H11B	109.5
C8—C2—C1	113.1 (5)	H11A—C11—H11B	109.5
N2—C2—C3	109.3 (5)	S2—C11—H11C	109.5
C8—C2—C3	104.4 (5)	H11A—C11—H11C	109.5
C1—C2—C3	114.6 (5)	H11B—C11—H11C	109.5
C4—C3—C5	107.6 (5)	S2—C12—H12A	109.5
C4—C3—C6	107.5 (5)	S2—C12—H12B	109.5
C5—C3—C6	116.0 (5)	H12A—C12—H12B	109.5
C4—C3—C2	109.2 (5)	S2—C12—H12C	109.5
C5—C3—C2	114.1 (5)	H12A—C12—H12C	109.5
C6—C3—C2	102.2 (5)	H12B—C12—H12C	109.5

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1NA···Cl3	0.92	2.35	3.223 (6)	160
N1—H1NB···O1	0.92	2.35	2.928 (7)	121
N1—H1NB···Cl1^i	0.92	2.82	3.599 (7)	144
N2—H2NB···O1^ii	0.92	2.16	2.982 (6)	147

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