Tetra-pyrazine-platinum(II) bis-(tetra-fluoro-borate) acetonitrile hemisolvate.

The improved synthesis and characterization of tetra-pyrazine-platinum(II) bis-(tetra-fluoro-borate) acetonitrile hemisolvate, [Pt(C(4)H(4)N(2))(4)](BF(4))(2)·0.5CH(3)CN, is reported. The unit cell contains a half equivalent of an acetonitrile solvent mol-ecule per tetra-pyrazine-platinum(II) ion. The coordination geometry of the Pt(II) ion is almost square-planar, with the Pt atom residing on an inversion center. The BF(4) (-) counter-anion, located at a general position, has an idealized tetra-hedral geometry and an acetonitrile solvent mol-ecule, the methyl group of which is disordered over two equal positions, sits on a twofold rotation axis.

Related literature

For general background, see: Derossi et al. (2007 ▶); Klika et al. (2007 ▶); Pearson et al. (1960 ▶); Schweiger et al. (2001 ▶); Wendt et al. (1997 ▶); Willermann et al. (2006 ▶). For related structures, see: Wei et al. (1989 ▶).

Experimental

Crystal data

[Pt(C4H4N2)4](BF4)2·0.5C2H3N

M = 709.6

Monoclinic,

a = 13.862 (4) Å

b = 10.819 (3) Å

c = 17.262 (5) Å

β = 91.607 (3)°

V = 2587.8 (13) Å3

Z = 4

Mo Kα radiation

μ = 5.50 mm−1

T = 296 (2) K

0.27 × 0.21 × 0.19 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2004 ▶) T min = 0.246, T max = 0.352

11212 measured reflections

2736 independent reflections

1846 reflections with I > 2σ(I)

R int = 0.039

Refinement

R[F 2 > 2σ(F 2)] = 0.033

wR(F 2) = 0.114

S = 1.20

2736 reflections

167 parameters

2 restraints

H-atom parameters constrained

Δρmax = 1.58 e Å−3

Δρmin = −0.45 e Å−3

Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶) and PLATON (Spek, 2003 ▶); software used to prepare material for publication: SHELXL97 and WinGX (Farrugia, 1999 ▶).

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808033679/pk2119sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808033679/pk2119Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Pt(C4H4N2)4](BF4)2·0.5C2H3N	F(000) = 1356
Mr = 709.6	Dx = 1.821 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 8501 reflections
a = 13.862 (4) Å	θ = 2.3–27.8°
b = 10.819 (3) Å	µ = 5.50 mm−1
c = 17.262 (5) Å	T = 296 K
β = 91.607 (3)°	Block, pale yellow
V = 2587.8 (13) Å3	0.27 × 0.21 × 0.19 mm
Z = 4

Bruker APEXII CCD diffractometer	1846 reflections with I > 2σ(I)
ω scans	Rint = 0.039
Absorption correction: multi-scan (SADABS; Bruker, 2004)	θmax = 26.7°, θmin = 2.4°
Tmin = 0.246, Tmax = 0.352	h = −17→17
11212 measured reflections	k = −13→13
2736 independent reflections	l = −21→21

Refinement on F2	2 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.033	w = 1/[σ2(Fo2) + (0.0518P)2 + 10.4546P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.114	(Δ/σ)max = 0.012
S = 1.20	Δρmax = 1.58 e Å−3
2736 reflections	Δρmin = −0.45 e Å−3
167 parameters

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.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Pt1	0	0.5	0	0.04102 (14)
N1	0.0732 (4)	0.5078 (5)	0.1031 (4)	0.0463 (13)
N2	0.1147 (4)	0.4171 (5)	−0.0466 (3)	0.0435 (13)
N3	0.1705 (8)	0.5173 (9)	0.2459 (5)	0.090 (3)
N4	0.2743 (5)	0.3006 (7)	−0.1078 (4)	0.0693 (19)
C1	0.1234 (7)	0.6071 (9)	0.1267 (5)	0.072 (3)
H1A	0.1267	0.6756	0.0943	0.087*
C2	0.1699 (8)	0.6096 (12)	0.1971 (6)	0.092 (3)
H2A	0.2031	0.6811	0.2113	0.11*
C3	0.1246 (7)	0.4181 (12)	0.2223 (5)	0.081 (3)
H3A	0.1257	0.3491	0.2545	0.097*
C4	0.0729 (6)	0.4100 (8)	0.1496 (5)	0.060 (2)
H4A	0.04	0.3383	0.1352	0.072*
C5	0.1983 (6)	0.4785 (6)	−0.0567 (5)	0.0509 (19)
H5A	0.2027	0.5615	−0.043	0.061*
C6	0.2764 (6)	0.4203 (9)	−0.0868 (5)	0.066 (2)
H6A	0.3329	0.465	−0.093	0.079*
C7	0.1921 (7)	0.2422 (8)	−0.0975 (5)	0.063 (2)
H7A	0.1881	0.1592	−0.1112	0.076*
C8	0.1128 (6)	0.2975 (7)	−0.0678 (5)	0.058 (2)
H8A	0.0566	0.2518	−0.0622	0.07*
B1	0.1048 (10)	0.1540 (11)	0.4316 (8)	0.081 (3)
F1	0.1311 (10)	0.1855 (9)	0.5039 (6)	0.226 (6)
F2	0.1324 (7)	0.2427 (8)	0.3805 (6)	0.163 (4)
F3	0.0102 (6)	0.1483 (9)	0.4290 (6)	0.172 (4)
F4	0.1480 (6)	0.0465 (7)	0.4153 (5)	0.125 (3)
N1S	0	0.224 (3)	−0.25	0.174 (15)*	0.5
C1S	0	0.124 (3)	−0.25	0.093 (9)*	0.5
C2S	0	−0.014 (3)	−0.25	0.16 (2)*	0.5
H2S1	0.039	−0.0435	−0.207	0.241*	0.25
H2S2	0.0259	−0.0435	−0.2976	0.241*	0.25
H2S3	−0.0649	−0.0435	−0.2454	0.241*	0.25

	U11	U22	U33	U12	U13	U23
Pt1	0.0407 (2)	0.0471 (2)	0.0350 (2)	0.00181 (19)	−0.00349 (13)	−0.00503 (18)
N1	0.045 (3)	0.053 (3)	0.041 (3)	0.007 (3)	−0.003 (2)	−0.006 (3)
N2	0.045 (3)	0.049 (3)	0.037 (3)	0.004 (3)	−0.003 (2)	0.002 (2)
N3	0.092 (7)	0.128 (9)	0.049 (5)	−0.012 (5)	−0.026 (4)	−0.011 (5)
N4	0.054 (4)	0.081 (5)	0.073 (5)	0.015 (4)	0.003 (3)	−0.014 (4)
C1	0.082 (6)	0.074 (6)	0.060 (5)	−0.027 (5)	−0.016 (5)	−0.004 (4)
C2	0.101 (8)	0.111 (9)	0.062 (6)	−0.038 (7)	−0.028 (6)	−0.007 (6)
C3	0.080 (6)	0.108 (9)	0.053 (5)	0.021 (6)	−0.004 (5)	0.013 (6)
C4	0.063 (5)	0.062 (5)	0.055 (5)	0.006 (4)	−0.016 (4)	0.004 (4)
C5	0.047 (4)	0.047 (5)	0.058 (5)	0.000 (3)	−0.001 (3)	−0.001 (3)
C6	0.046 (4)	0.080 (6)	0.072 (6)	0.002 (4)	0.005 (4)	0.001 (5)
C7	0.074 (6)	0.049 (5)	0.066 (5)	0.016 (4)	−0.004 (4)	−0.013 (4)
C8	0.061 (5)	0.052 (4)	0.062 (5)	−0.004 (4)	0.000 (4)	−0.012 (4)
B1	0.091 (9)	0.064 (7)	0.088 (9)	0.024 (6)	−0.018 (7)	−0.003 (6)
F1	0.329 (15)	0.179 (9)	0.166 (9)	0.089 (9)	−0.080 (10)	−0.091 (8)
F2	0.192 (9)	0.109 (6)	0.188 (9)	0.034 (6)	0.032 (7)	0.062 (6)
F3	0.088 (5)	0.200 (9)	0.227 (11)	0.021 (6)	−0.015 (6)	0.031 (7)
F4	0.172 (8)	0.073 (3)	0.131 (6)	0.050 (5)	−0.001 (5)	−0.006 (4)

Pt1—N2i	2.012 (5)	C4—H4A	0.93
Pt1—N2	2.012 (5)	C5—C6	1.368 (11)
Pt1—N1i	2.026 (6)	C5—H5A	0.93
Pt1—N1	2.026 (6)	C6—H6A	0.93
N1—C4	1.327 (10)	C7—C8	1.364 (11)
N1—C1	1.337 (10)	C7—H7A	0.93
N2—C8	1.345 (9)	C8—H8A	0.93
N2—C5	1.352 (9)	B1—F3	1.312 (14)
N3—C3	1.307 (14)	B1—F1	1.335 (14)
N3—C2	1.307 (13)	B1—F4	1.342 (12)
N4—C7	1.319 (11)	B1—F2	1.365 (14)
N4—C6	1.344 (11)	N1S—C1S	1.086 (14)
C1—C2	1.360 (12)	C1S—C2S	1.492 (10)
C1—H1A	0.93	C2S—H2S1	0.96
C2—H2A	0.93	C2S—H2S2	0.96
C3—C4	1.432 (12)	C2S—H2S3	0.96
C3—H3A	0.93
N2i—Pt1—N2	180.0 (3)	N2—C5—C6	120.9 (7)
N2i—Pt1—N1i	89.3 (2)	N2—C5—H5A	119.6
N2—Pt1—N1i	90.7 (2)	C6—C5—H5A	119.6
N2i—Pt1—N1	90.7 (2)	N4—C6—C5	122.3 (8)
N2—Pt1—N1	89.3 (2)	N4—C6—H6A	118.8
N1i—Pt1—N1	180.00 (18)	C5—C6—H6A	118.8
C4—N1—C1	117.9 (7)	N4—C7—C8	123.3 (8)
C4—N1—Pt1	119.2 (5)	N4—C7—H7A	118.4
C1—N1—Pt1	123.0 (5)	C8—C7—H7A	118.4
C8—N2—C5	116.6 (6)	N2—C8—C7	121.0 (8)
C8—N2—Pt1	121.9 (5)	N2—C8—H8A	119.5
C5—N2—Pt1	121.5 (5)	C7—C8—H8A	119.5
C3—N3—C2	115.6 (9)	F3—B1—F1	106.8 (12)
C7—N4—C6	115.9 (7)	F3—B1—F4	113.9 (12)
N1—C1—C2	121.1 (9)	F1—B1—F4	107.8 (10)
N1—C1—H1A	119.4	F3—B1—F2	108.0 (10)
C2—C1—H1A	119.4	F1—B1—F2	110.5 (12)
N3—C2—C1	123.8 (10)	F4—B1—F2	109.8 (11)
N3—C2—H2A	118.1	N1S—C1S—C2S	180.000 (5)
C1—C2—H2A	118.1	C1S—C2S—H2S1	109.5
N3—C3—C4	123.4 (10)	C1S—C2S—H2S2	109.5
N3—C3—H3A	118.3	H2S1—C2S—H2S2	109.5
C4—C3—H3A	118.3	C1S—C2S—H2S3	109.5
N1—C4—C3	118.1 (8)	H2S1—C2S—H2S3	109.5
N1—C4—H4A	120.9	H2S2—C2S—H2S3	109.5
C3—C4—H4A	120.9