Di­chloro­bis­(pheno­thia­zine-κS)­palladium(II)

In the title complex, [PdCl₂(C₁₂H₉NS)₂], the Pd atom lies on a center of inversion and is coordinated by two chloride anions and two S atoms from two pheno­thia­zine ligands, forming a square-planar PdCl₂S₂ geometry. In the crystal structure, a one-dimensional polymer structure is constructed via N—H...Cl and N—H...N hydrogen bonds.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.024
• wR factor = 0.065
• Data-to-parameter ratio = 17.8

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT417_ALERT_2_B Short Inter D-H..H-D       H1     ..  H1      ..       2.05 Ang.

Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.98
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large .............       0.88
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Pd1    -   Cl1     ..       7.67 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Pd1    -   S1      ..       5.27 su

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

   0 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
   2 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Dichlorobis(phenothiazine-κS)palladium(II)

Crystal data

[PdCl2(C12H9NS)2]	Z = 1
Mr = 575.82	F(000) = 288
Triclinic, P1	Dx = 1.699 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.6036 (5) Å	Cell parameters from 3594 reflections
b = 8.8540 (5) Å	θ = 2.4–27.8°
c = 8.9240 (5) Å	µ = 1.26 mm^−1
α = 70.985 (1)°	T = 295 K
β = 82.297 (1)°	Block, brown
γ = 86.860 (1)°	0.25 × 0.24 × 0.20 mm
V = 562.84 (6) Å^3

Data collection

Bruker APEX area-detector diffractometer	2526 independent reflections
Radiation source: fine-focus sealed tube	2416 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.015
φ and ω scans	θmax = 27.5°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Bruker, 2002)	h = −9→9
Tmin = 0.659, Tmax = 0.786	k = −11→11
4874 measured reflections	l = −11→11

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.065	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0423P)^2 + 0.0826P] where P = (Fo^2 + 2Fc^2)/3
2526 reflections	(Δ/σ)max = 0.001
142 parameters	Δρmax = 0.30 e Å^−3
0 restraints	Δρmin = −0.50 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pd1	0.5000	0.5000	0.5000	0.02986 (8)
Cl1	0.40055 (7)	0.25433 (5)	0.67039 (6)	0.04237 (12)
S1	0.22282 (6)	0.59164 (5)	0.58532 (6)	0.03352 (11)
N1	0.3365 (2)	0.90820 (19)	0.6082 (2)	0.0373 (3)
H1	0.4085	0.9832	0.5989	0.045*
C1	0.2582 (2)	0.6331 (2)	0.7602 (2)	0.0347 (4)
C2	0.2318 (3)	0.5112 (3)	0.9052 (3)	0.0477 (5)
H2	0.1891	0.4130	0.9101	0.057*
C3	0.2694 (4)	0.5366 (3)	1.0423 (3)	0.0609 (7)
H3	0.2514	0.4557	1.1401	0.073*
C4	0.3335 (3)	0.6822 (3)	1.0337 (3)	0.0547 (6)
H4	0.3618	0.6979	1.1257	0.066*
C5	0.3562 (3)	0.8046 (3)	0.8909 (3)	0.0455 (5)
H5	0.3972	0.9028	0.8875	0.055*
C6	0.3179 (2)	0.7822 (2)	0.7501 (2)	0.0348 (4)
C7	0.2450 (2)	0.9199 (2)	0.4802 (2)	0.0331 (4)
C8	0.2177 (3)	1.0687 (2)	0.3687 (3)	0.0423 (4)
H8	0.2639	1.1598	0.3781	0.051*
C9	0.1221 (3)	1.0808 (3)	0.2439 (3)	0.0515 (5)
H9	0.1060	1.1805	0.1692	0.062*
C10	0.0500 (3)	0.9477 (3)	0.2282 (3)	0.0515 (5)
H10	−0.0164	0.9579	0.1451	0.062*
C11	0.0773 (3)	0.7995 (3)	0.3369 (2)	0.0426 (4)
H11	0.0290	0.7092	0.3275	0.051*
C12	0.1774 (2)	0.7853 (2)	0.4607 (2)	0.0331 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pd1	0.03285 (12)	0.02316 (11)	0.03767 (12)	−0.00027 (7)	−0.00666 (8)	−0.01447 (8)
Cl1	0.0466 (3)	0.0267 (2)	0.0531 (3)	−0.00279 (19)	−0.0008 (2)	−0.0136 (2)
S1	0.0325 (2)	0.0263 (2)	0.0442 (2)	−0.00182 (17)	−0.00465 (18)	−0.01442 (18)
N1	0.0392 (8)	0.0283 (8)	0.0470 (9)	−0.0062 (6)	−0.0077 (7)	−0.0136 (7)
C1	0.0339 (9)	0.0334 (9)	0.0379 (9)	0.0022 (7)	−0.0024 (7)	−0.0140 (7)
C2	0.0561 (13)	0.0380 (11)	0.0448 (11)	−0.0024 (9)	0.0027 (9)	−0.0106 (9)
C3	0.0766 (18)	0.0600 (15)	0.0373 (11)	0.0066 (13)	−0.0018 (11)	−0.0069 (10)
C4	0.0603 (14)	0.0673 (16)	0.0417 (11)	0.0105 (12)	−0.0117 (10)	−0.0246 (11)
C5	0.0478 (11)	0.0486 (12)	0.0492 (12)	0.0048 (9)	−0.0121 (9)	−0.0266 (10)
C6	0.0299 (8)	0.0359 (10)	0.0411 (10)	0.0025 (7)	−0.0046 (7)	−0.0160 (8)
C7	0.0308 (8)	0.0304 (9)	0.0386 (9)	0.0023 (7)	−0.0026 (7)	−0.0128 (7)
C8	0.0419 (10)	0.0313 (9)	0.0497 (11)	0.0025 (8)	−0.0003 (9)	−0.0102 (8)
C9	0.0495 (12)	0.0472 (12)	0.0453 (11)	0.0110 (10)	−0.0037 (9)	−0.0009 (9)
C10	0.0470 (12)	0.0624 (15)	0.0441 (11)	0.0097 (10)	−0.0124 (9)	−0.0148 (10)
C11	0.0377 (10)	0.0504 (12)	0.0461 (11)	0.0025 (8)	−0.0092 (8)	−0.0228 (9)
C12	0.0287 (8)	0.0315 (9)	0.0399 (9)	0.0023 (7)	−0.0029 (7)	−0.0136 (7)

Geometric parameters (Å, º)

Pd1—Cl1	2.3091 (5)	C4—C5	1.375 (3)
Pd1—Cl1^i	2.3091 (5)	C4—H4	0.9300
Pd1—S1	2.3378 (5)	C5—C6	1.403 (3)
Pd1—S1^i	2.3378 (5)	C5—H5	0.9300
S1—C12	1.758 (2)	C7—C12	1.393 (3)
S1—C1	1.772 (2)	C7—C8	1.392 (3)
N1—C6	1.385 (2)	C8—C9	1.382 (3)
N1—C7	1.389 (2)	C8—H8	0.9300
N1—H1	0.8600	C9—C10	1.382 (4)
C1—C6	1.391 (3)	C9—H9	0.9300
C1—C2	1.387 (3)	C10—C11	1.378 (3)
C2—C3	1.382 (3)	C10—H10	0.9300
C2—H2	0.9300	C11—C12	1.393 (3)
C3—C4	1.379 (4)	C11—H11	0.9300
C3—H3	0.9300
Cl1—Pd1—Cl1^i	180	C4—C5—C6	120.4 (2)
Cl1—Pd1—S1	84.05 (2)	C4—C5—H5	119.8
Cl1—Pd1—S1^i	95.95 (2)	C6—C5—H5	119.8
Cl1^i—Pd1—S1^i	84.05 (2)	C1—C6—N1	122.44 (17)
Cl1^i—Pd1—S1	95.95 (2)	C1—C6—C5	117.94 (18)
S1—Pd1—S1^i	180	N1—C6—C5	119.61 (18)
C12—S1—C1	100.27 (9)	N1—C7—C12	121.39 (16)
C12—S1—Pd1	110.94 (6)	N1—C7—C8	120.00 (17)
C1—S1—Pd1	103.66 (6)	C12—C7—C8	118.61 (17)
C6—N1—C7	123.50 (16)	C9—C8—C7	120.0 (2)
C6—N1—H1	118.2	C9—C8—H8	120.0
C7—N1—H1	118.2	C7—C8—H8	120.0
C6—C1—C2	121.40 (19)	C10—C9—C8	121.2 (2)
C6—C1—S1	120.39 (15)	C10—C9—H9	119.4
C2—C1—S1	118.16 (16)	C8—C9—H9	119.4
C3—C2—C1	119.5 (2)	C9—C10—C11	119.4 (2)
C3—C2—H2	120.2	C9—C10—H10	120.3
C1—C2—H2	120.2	C11—C10—H10	120.3
C4—C3—C2	119.8 (2)	C10—C11—C12	119.9 (2)
C4—C3—H3	120.1	C10—C11—H11	120.1
C2—C3—H3	120.1	C12—C11—H11	120.1
C5—C4—C3	120.9 (2)	C7—C12—C11	120.83 (18)
C5—C4—H4	119.6	C7—C12—S1	121.47 (14)
C3—C4—H4	119.6	C11—C12—S1	117.64 (15)
Cl1—Pd1—S1—C12	−166.02 (7)	C4—C5—C6—C1	−0.5 (3)
Cl1^i—Pd1—S1—C12	13.98 (7)	C4—C5—C6—N1	178.0 (2)
Cl1—Pd1—S1—C1	87.15 (7)	C6—N1—C7—C12	−22.9 (3)
Cl1^i—Pd1—S1—C1	−92.85 (7)	C6—N1—C7—C8	156.52 (18)
C12—S1—C1—C6	−26.79 (17)	N1—C7—C8—C9	−178.07 (18)
Pd1—S1—C1—C6	87.90 (15)	C12—C7—C8—C9	1.4 (3)
C12—S1—C1—C2	155.80 (16)	C7—C8—C9—C10	0.9 (3)
Pd1—S1—C1—C2	−89.51 (16)	C8—C9—C10—C11	−1.5 (3)
C6—C1—C2—C3	−1.6 (3)	C9—C10—C11—C12	−0.2 (3)
S1—C1—C2—C3	175.8 (2)	N1—C7—C12—C11	176.36 (17)
C1—C2—C3—C4	−0.3 (4)	C8—C7—C12—C11	−3.1 (3)
C2—C3—C4—C5	1.8 (4)	N1—C7—C12—S1	−6.4 (2)
C3—C4—C5—C6	−1.4 (4)	C8—C7—C12—S1	174.18 (14)
C2—C1—C6—N1	−176.54 (17)	C10—C11—C12—C7	2.5 (3)
S1—C1—C6—N1	6.1 (3)	C10—C11—C12—S1	−174.83 (16)
C2—C1—C6—C5	1.9 (3)	C1—S1—C12—C7	27.04 (17)
S1—C1—C6—C5	−175.38 (15)	Pd1—S1—C12—C7	−82.01 (15)
C7—N1—C6—C1	23.0 (3)	C1—S1—C12—C11	−155.62 (15)
C7—N1—C6—C5	−155.45 (18)	Pd1—S1—C12—C11	95.34 (14)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···Cl1^ii	0.86	2.67	3.359 (2)	138
N1—H1···N1^iii	0.86	2.49	3.109 (2)	130

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